Category: 4090-55-5

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, This compound has unique chemical properties. The synthetic route is as follows., 4090-55-5

Into a 250mL reaction vessel which is equipped with a stirrer and cooling device, add 18.40 g of 2,2-dimethyl-1,3-propanediol-phosphonoyl chloride (0.1mol) and 50mL of tetrahydrofuran, open the stir for the solution dissolve evenly; at below 0-10 C stirring slowly and added the drops of diethanolamine (0.1mol,10 ? 51 g), triethylamine (0.3 mol, 30.36 g) as well as 100mL of tetrahydrofuran solution, the system gradually produces white precipitates.The solution is added drop-wise after that, the system is allowed to react at 0-10 C for 10 hours, and then heated at 20 C reaction for 12 hours, the white precipitated triethylamine hydrochloride is filtered after that concentrated under reduced pressure, purification and drying and then obtained light yellow transparent oily liquid product, yield is 98.5%.

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Reference:
Patent; North University of China; Zhao Bin; Liu Yaqing; Li Fei; Xiong Kuankuan; Wang Xiaofeng; Liu Xueyi; (10 pag.)CN104892676; (2017); B;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

4090-55-5, The chemical industry reduces the impact on the environment during synthesis 4090-55-5, name is 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide, I believe this compound will play a more active role in future production and life.

To a stirred solution of S2 (0.84 g, 1.50 mmol) in THF (5 mL) at rt, 60%NaH (0.24 g, 6.0 mmol) was added and stirred for 30 min. Then 2,2-dimethyltrimethylene phosphorochloridate (0.39 g, 2.2 mmol) was added in one portion. After stirring for 9 hours at rt, the reaction was quenched by saturated aqueous NaHCO3 and extracted with EtOAc. The organic layer was washed with water and brine and dried over MgSO4. After filtration, the reaction mixture was concentrated in vacuo and the crude product was purified by column chromatography to give 1c as colorless foam in 85% yield (0.90 g, 1.3 mmol). 4-Fluorophenyl 3,4,6-tri-O-benzyl-2-O-(2,2-dimethyltrimethylenephosphornoyl)-1-thio-alpha-D-mannopyranoside (1c). TLC (hexane/EtOAc 5:3):Rf 0.50. [alpha]D = +76.8 (c = 1.1, CHCl3). 1H NMR (CDCl3, 600 MHz) 7.45 (dd, J= 9.0, 5.4 Hz, 2 H), 7.41 – 7.40 (m, 2 H), 7.35 – 7.27 (m, 11 H), 7.25 – 7.23 (m, 2H), 6.94 (pseudo-t, J = 9.0 Hz, 2 H), 5.59 (d, J = 1.8 Hz, 1 H), 5.11 (dt, J = 7.8,2.4 Hz), 4.91 (d, J = 10.8 Hz, 1 H), 4.82 (d, J = 11.4 Hz, 1 H), 4.63 (d, J = 11.4Hz, 1 H), 4.62 (d, J = 11.4 Hz, 1 H), 4.59 (d, J = 10.8 Hz, 1 H), 4.48 (d, J = 12.0Hz, 1 H), 4.33 (ddd, J = 5.4, 4.2, 3.0 Hz, 1 H), 4.14 (d, J = 10.8 Hz, 1 H), 4.09 (d,J = 10.8 Hz, 1 H), 3.96 (pseudo-t, J = 9.6 Hz, 1 H), 3.91 – 3.85 (m, 2 H), 3.76(ddd, J = 21.6, 10.8, 3.0 Hz, 1 H) 3.75 (dd, J = 10.8, 3.0 Hz, 1 H) 3.67 (ddd, J =22.2, 11.4, 3.0 Hz, 1 H), 1.22 (s, 3 H), 0.63 (s, 3 H). 13C NMR (CDCl3, 150 MHz) 162.8 (d, J = 246.9 Hz), 138.2, 138.0, 137.4, 134.9 (d, J = 8.1 Hz), 128.5,128.4, 128.36, 128.34, 128.2 (d, J = 3.3 Hz), 128.1, 128.0, 127.9, 127.6, 116.2 (d,J = 21.9 Hz), 87.4, 79.1, 78.39, 78.35, 78.30, 78.25, 78.1, 75.2, 74.4, 74.3, 74.1,73.4, 72.6, 71.9, 69.0, 32.0, 21.8, 20.1. HRMS (ESI) m/z calcd for C38H42FNNaO8PS [M+Na]+, 731.2214; found, 731.2223.

The chemical industry reduces the impact on the environment during synthesis 2-Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane 2-oxide. I believe this compound will play a more active role in future production and life.

Reference:
Article; Manmode, Sujit; Sato, Takumi; Sasaki, Norihiko; Notsu, Ikumi; Hayase, Shuichi; Nokami, Toshiki; Itoh, Toshiyuki; Carbohydrate Research; vol. 450; (2017); p. 44 – 48;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics