Category: 772-49-6

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 772-49-6, name is 1-Chloro-3-(trifluoromethoxy)benzene, A new synthetic method of this compound is introduced below., category: chlorides-buliding-blocks

To a cooed (-78 C) soution of 1-choro-3-(trifluoromethoxy)benzene (100 g, 510 mmo)in THF (500 mL) was added n-butyflithium (2.5 M/hexanes, 205 mL, 510 mmo)dropwise over a period of 10 minutes. Stirring was maintained at -78 C for I h, andthen a soution of iodine (130 g, 510 mmo) in THF (500 mL) was added dropwise at -78C over a period of 30 minutes. After the addition, the temperature was maintained at -78 C for lh and then aflowed to warm to rt and stirred for a tota? of 18h. The reaction mixture was poured into saturated aqueous Na2SO3 and extracted with EtOAc (2 x 1000 mL). The combined organic extracts were dried over Na2SO4 and concentrated in vacuo to give the tifle compound as an oH (159 g, 96% yied). 1H NMR (500 MHz, CDC3) 67.40 (dd, J= 8.1, 1.4 Hz. IH), 7.32 (t, J= 8.1 Hz, IH). 7.16(dt. J= 8.2, 1.4 Hz, IH).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; RAVULA, Suchitra; SWANSON, Devin M.; SAVALL, Bradley M.; AMERIKS, Michael K.; (250 pag.)WO2016/176449; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 772-49-6, name is 1-Chloro-3-(trifluoromethoxy)benzene, A new synthetic method of this compound is introduced below., COA of Formula: C7H4ClF3O

N,N-Di-isopropylamine (38.4 ml, 27lmmol) was added dropwise to a solution of nbutyllithium (1.6 M, 169 ml, 271 mmol) in THF (180 ml) at 0C and the reaction mixture was stirred and allowed to warm to room temperature over 30 mins. The LDA solution was then added drop wise over lOminutes to a solution of 1-chloro-3- (trifluoromethoxy)benzene (50 g, 246 mmol) in THF (500 ml) at -70C and the resultingmixture was stirred at -70C for 30 minutes. Finally N,N-dimethylformamide (23 ml, 296 mmol) was added dropwise and the resultant mixture stirred at -70C for 30 minutes.The reaction was quenched at -70C by addition of NH4C1 (saturated aqueous solution) to pH 7-8 and the resulting mixture was extracted with EtOAc (3 x 75 ml). The combined organic phases were washed with water (100 ml), brine (100 ml), dried over magnesium sulfate, filtered and concentrated under reduced pressure to provide the title compound (55 g, 99% yield).LCMS (Method 16, ES+) RT 1.32 mm., 224 [M+H].

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; UCB BIOPHARMA SPRL; SANOFI; DE HARO GARCIA, Teresa; DELIGNY, Michael; HEER, Jag Paul; QUINCEY, Joanna Rachel; XUAN, Mengyang; ZHU, Zhaoning; BROOKINGS, Daniel Christopher; CALMIANO, Mark Daniel; EVRARD, Yves; HUTCHINGS, Martin Clive; JOHNSON, James Andrew; JADOT, Sophie; KEYAERTS, Jean; MAC COSS, Malcolm; SELBY, Matthew Duncan; SHAW, Michael Alan; SWINNEN, Dominique Louis Leon; SCHIO, Laurent; FORICHER, Yann; FILOCHE-ROMME, Bruno; (365 pag.)WO2016/50975; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

772-49-6, A common heterocyclic compound, 772-49-6, name is 1-Chloro-3-(trifluoromethoxy)benzene, molecular formula is C7H4ClF3O, 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.

To a cooed (-.78 C) souUon of 1-choro-3-(trfluoromethoxy)benzene (20 g, 102 mrno)n THF (100 mL) was added n-butyWthum (2.5 M/hexanes, 41 mL, 102 mmo) dropwseover a period of 10 minutes. Strrng was mantaned at -78C for I h, and then asouDon of odne (26 g, 102 rnrno) n THF (100 mL) was added dropwse at -.78 C overa perod of 30 ninutes. After the add Won, the temperature was niantaned at -78 C for1 h and then aflowed to warm to rt and stirred for a tota of 18 h. The reacton mixturewas poured nto saturated aqueous Na2SO3 and extracted wfth EtOAc (2 x 200 mL). The combined organc extracts were dried over Na2SO4 and concentrated n vacuo to give the tWe compound as an oH (28 g, 85% yed). 1H NMR (500 MHz, CDC3) oe 7.40 (dd, J = 81, 1.4 Hz, IH), 7.32 (t, J = 8.1 Hz, IH), 7.16 (dt, J = 8.2, 1.4 Hz, IH).

The synthetic route of 772-49-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; JANSSEN PHARMACEUTICA NV; AMERIKS, Michael K.; RAVULA, Suchitra; SAVALL, Bradley M.; SWANSON, Devin M.; ZIFF, Jeannie M.; SHIREMAN, Brock T.; (167 pag.)WO2016/176463; (2016); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics