Category: 56961-77-4

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 56961-77-4 as follows. Quality Control of 1-Bromo-2,3-dichlorobenzene

Under a nitrogen atmosphere, and added at 80 will have diphenylamine (37.5g),1- bromo-2,3-dichlorobenzene (50.0g), Pd-132 (Johnson Matthey) (0.8 g of ), NaOtBu(32.0g) and xylene (500ml) was heated in a flask and stirred for 4 hours, the temperature was raised to 120 up, and further heated with stirring for 3 hours. Thereaction mixture was cooled until room temperature, water and ethyl acetate to carry outa liquid. Then, the use of silica gel column chromatography (eluent: toluene / heptane =1/20 (volume ratio)) to be purified, is obtained 2,3-dichloro -N, N- diphenyl aniline(63.0g) .

According to the analysis of related databases, 56961-77-4, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Kwansei Gakuin School Corporation; Tian, Shanzuoci; Zhong, Zhongzongyiliang; Zhong, Daoguiyi; Ping, Jingdagui; Xiao, Yeyangping; Zhi, Lianyizhi; Ni, Jingping; Song, Xiawusi; Sheng, Tianlizhao; (405 pag.)CN105431439; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 56961-77-4, These common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Intermediate 1:[0114] A well-dried flask was first charged with l-bromo-2,3-dichlorobenzene (4 g, 17.7 mmol) and 1,4-diazepane (2.1 g, 20.9 mmol), which was evacuated and backfilled with N2 through a balloon under gentle warming (40C). Toluene was charged and the mixture was bubbled with N2 for 10 min, then BINAP (318 mg, 0.51 mmol) and Pd2dba3 (156 mg, 0.17 mmol) was added to the mixture, followed by DBU (3.4 mL). The resulting mixture was warmed at 60- 70C while fine powder of tBuONa was added in one portion to start the amination. After the reaction mixture cooled to rt, (Boc)20 (11 g, 51 mmol) solution in DCM was added dropwise to the reaction mixture, then stirred for 3 h at rt. The reaction mixture was diluted with water and extracted with EtOAc. The combined EtOAc layers were washed with brine, dried over anhydrous Na2S04, concentrated in vacuo and purified by flash chromatography on silica gel column (elution with PE/EtOAc = 10:1) to give tert-butyl 4-(2,3-dichlorophenyl)-l,4-diazepane- 1-carboxylate (intermediate 1) (4.1 g, 70%) as a yellow oil.

Statistics shows that 1-Bromo-2,3-dichlorobenzene is playing an increasingly important role. we look forward to future research findings about 56961-77-4.

Reference:
Patent; THE UNIVERSITY OF NORTH CAROLINA AT CHAPEL HILL; JIN, Jian; ROTH, Bryan; FRYE, Stephen; WO2012/3418; (2012); A2;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Reference of 56961-77-4, A common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Intermediate 1-1 was synthesized according to the following reaction formula. To a 2 L flask was added 1-bromo-2,3-dichlorobenzene (55.0 g, 0.243 mol) and sodium tert-butoxide (72.5 g, 0.755 mol) with 700 mL of toluene and the mixture was refluxed for one hour and stirred. After cooling to room temperature, aniline (45.1 g, 0.485 mol) was added and the temperature was raised. After adding 2,2′-bis (diphenylphosphino) -1,1′-binaphthalene (rac-BINAP) (6.06 g, 9.74 mmole), tris (dibenzylideneacetone) dipalladium (0) (4.46 g, 0.284 mol) dissolved in 30 mL of toluene was slowly added dropwise. After completion of the reaction, the reaction mixture was cooled to room temperature, extracted with ethyl acetate and water, and the obtained organic layer was treated with anhydrous magnesium sulfate, filtered and concentrated to obtain the desired product. Intermediate 1-1 (36.0 g, yield 50%) was obtained by column chromatography using ethyl acetate and hexane.

The synthetic route of 56961-77-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; LG Chem, Ltd.; Gu Gi-dong; Lee Gi-gon; Kim Gong-gyeom; Kim Hyeong-seok; Hwang Seong-seok; Lee Sang-u; (28 pag.)KR2019/37174; (2019); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 56961-77-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 56961-77-4 name is 1-Bromo-2,3-dichlorobenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

To 1-bromo-2,3-dichlorobenzene [r-1] (22.6 g, 100 mmol), sodium t-butoxide (29.6 g, 308 mmol), 2,2?-bis (diphenylphosphino)-1 , 1 ?-binaphthyl [I3INAP] (2.51 g, 4.0 mmol), bis(dibenzylideneacetone) palladium (0) [Pd2 (dba) 31(1.83 g, 2.0 mmol), and toluene (400 ml), aniline [r-2] (18.5 ml, 203 mmol) was added under a nitrogen atmosphere at room temperature, and the resulting mixture was heated and stirred at 1000 C. for 26 hours. The reaction solution was cooled to room temperature, and was filtered using silica gel column chromatography, and a solvent was distilled oil under reduced pressure to obtain a crude product. Thereafier, the resulting crude product was washed with toluene to obtain 2-chloro-N,N?-diphenyl- 1 ,3-benzenediamine [r-3] (18.4 g, yield 63%) as a white solid. The structure of the compound thus obtained was identified with an NMR spectrum. 1H-NMR (400 MHz, CDC13): &6.08 (s, 2H), 6.80 (s, 2H), 6.99 (t, 1H), 7.04 (U, J=1.1, 7.3 Hz, 2H, (CH)2CH (CR2)2), 7.18 (dd, 4H), 7.32 (dd, 4H). 13C-NMR (101 MHz, CDC13): 107.1 (2C), 109.4,120.4 (4C), 122.5 (2C), 127.0, 129.3 (4C), 141.1 (2C), 141.6 (2C).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2,3-dichlorobenzene, and friends who are interested can also refer to it.

Reference:
Patent; Kwansei Gakuin Educational Foundation; JNC Corporation; Hatakeyama, Takuji; NAKATSUKA, Soichiro; GOTOH, Hajime; SASADA, Yasuyuki; YANAI, Motoki; IKUTA, Toshiaki; (337 pag.)US2018/69182; (2018); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 56961-77-4,Some common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Under a nitrogen atmosphere, and added at 120 will have the N 1 , the N 1 ,the N 3 – triphenyl benzene-1,3-diamine (20.0g), 1- bromo-2,3-dichlorobenzene ( 6.4g),Pd-132 (0.2g ), NaOtBu (6.8g) and xylene (70ml) was stirred for 2 hours the flask washeated. The reaction mixture was cooled until room temperature, water and ethyl acetateto carry out a liquid. Then, the use of silica gel column chromatography (eluent:toluene / heptane = 4/6 (volume ratio)) to be purified, to thereby obtain the N 1 , theN 1 ‘ – (2- chloro-1,3-phenylene yl) bis (the N 1 , the N 3 , the N 3 – phenyl-trityl-1,3-diamine) (15.0g)

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2,3-dichlorobenzene, its application will become more common.

Reference:
Patent; Kwansei Gakuin School Corporation; Tian, Shanzuoci; Zhong, Zhongzongyiliang; Zhong, Daoguiyi; Ping, Jingdagui; Xiao, Yeyangping; Zhi, Lianyizhi; Ni, Jingping; Song, Xiawusi; Sheng, Tianlizhao; (405 pag.)CN105431439; (2016); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Some common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. SDS of cas: 56961-77-4

EXAMPLE 10 6-(2,3-Dichlorophenyl)-1,2-dihydro-2,2,4-trimethylquinoline (Compound 109, structure 4 of Scheme II, where R1 =2,3-dichlorophenyl) This compound was prepared according to General Method 2 (EXAMPLE 9). From Compound 9 (68.0 mg, 0.21 mmol) and commercially available 2,3-dichlorobromobenzene (40.1 mg, 0.18 mmol, Lancaster) was obtained a crude product which was isolated and purified by reverse phase HPLC (ODS column, 97% methanol/water, 3.0 mL/min) to afford 20 mg (29%) of Compound 109. Data for Compound 109: 1 H-NMR (400 MHz, CDCl3)7.39(dd, J=8, 1.6, 1H), 7.19 (dd, J=16, 8, 1H), 7.23 (dd, J=4, 1.6, 1H), 7.11 (d, J=1.6, 1H), 7.05 (dd, J=8, 1.6, 1H), 6.46 (d, J=8, 1H), 5.34 (s, 1H), 3.82 (br s, 1H), 1.99 (s, 3H), 1.32 (s, 6H).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 56961-77-4, its application will become more common.

Reference:
Patent; Ligand Pharmaceuticals Incorporated; US5693647; (1997); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Related Products of 56961-77-4,Some common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

In a nitrogen atmosphere, a flask containing 60 N1,N1,N3-triphenylbenzene-1,3-diamine (20.0 g), 44 1-bromo-2,3-dichlorobenzene (6.4 g), Pd-132 (0.2 g), 45 NaOtBu (6.8 g), and 28 xylene (70 ml) was heated and stirred at 120 C. for two hours. The reaction liquid was cooled to room temperature. Thereafter, 30 water and 40 ethyl acetate were added thereto, and the resulting mixture was partitioned. Subsequently, purification was performed by silica gel column chromatography (eluent: toluene/heptane=4/6 (volume ratio)) to obtain 88 N1,N1?-(2-chloro-1,3-phenylene) bis(N1,N3,N3-triphenylbenzene-1,3-diamine) (15.0 g).

The synthetic route of 56961-77-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JNC CORPORATION; FUJITA, Yukihiro; (228 pag.)US2019/165279; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Application of 56961-77-4,Some common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

29.3 g (100.0 mmol) of Compound 1-A, 22.6 g (100.0 mmol) of Compound 1-B, 2.7 g (3.0 mmol) of Pd2(dba)3, 1.3 g (6.0 mmol) of PtBu3 (50% solution in toluene), 28.8 g (300.0 mmol) of NaOtBu were mixed with 1,500 mL of toluene under a nitrogen (N2) atmosphere, followed by stirring under reflux to allow a reaction to occur for 12 hours. At room temperature, an organic layer was separated therefrom using water and ethyl acetate, and the solvent was dried. Then, through silica gel column chromatography, 28.5 g of compound 49-C was obtained at a yield of 65%. [0352] MS (MALDI-TOF) m/z: 438 [M]+

The synthetic route of 56961-77-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Samsung Display Co., Ltd.; KIM, Myeongsuk; YE, Jimyoung; YOO, Byeongwook; JEONG, Jaeho; (102 pag.)US2020/98991; (2020); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Synthetic Route of 56961-77-4,Some common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

In a nitrogen atmosphere, a flask containing 60 N1,N1,N3-triphenylbenzene-1,3-diamine (51.7 g), 44 1-bromo-2,3-dichlorobenzene (35.0 g), Pd-132 (0.6 g), 45 NaOtBu (22.4 g), and 28 xylene (350 ml) was heated and stirred at 90 C. for two hours. The reaction liquid was cooled to room temperature. Thereafter, 30 water and 40 ethyl acetate were added thereto, and the resulting mixture was partitioned. Subsequently, purification was performed by silica gel column chromatography (eluent: toluene/heptane=5/5 (volume ratio)) to obtain 61 N1-(2,3-dichlorophenyl)-N1,N3,N3-triphenylbenzene-1,3-diamine (61.8 g).

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2,3-dichlorobenzene, its application will become more common.

Reference:
Patent; JNC CORPORATION; FUJITA, Yukihiro; (228 pag.)US2019/165279; (2019); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Electric Literature of 56961-77-4,Some common heterocyclic compound, 56961-77-4, name is 1-Bromo-2,3-dichlorobenzene, molecular formula is C6H3BrCl2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

29.3 g (100.0 mmol) of Compound 1-A, 10.3 g (45.5 mmol) of Compound 1-B, 2.5 g (2.7 mmol) of Pd2(dba)3, 1.2 g (5.5 mmol) of PtBu3 (50 percent (%) solution in toluene), 26.2 g (272.7 mmol) of NaOtBu were mixed with 1,000 milliliters (mL) of toluene under a nitrogen (N2) atmosphere, followed by stirring under reflux to allow a reaction to occur for 12 hours. At room temperature, an organic layer was separated therefrom using water and ethyl acetate, and the solvent was dried. Then, through silica gel column chromatography, 19.0 g of Compound 1-C was obtained at a yield of 60%. [0296] MS (MALDI-TOF) m/z: 695 [M]+

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1-Bromo-2,3-dichlorobenzene, its application will become more common.

Reference:
Patent; Samsung Display Co., Ltd.; KIM, Myeongsuk; YE, Jimyoung; YOO, Byeongwook; JEONG, Jaeho; (102 pag.)US2020/98991; (2020); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics