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ChemicalBook CAS DataBase List 1,3,2-Dioxaphospholane, 2-(2,2,2-trifluoroethoxy)-, 2-oxide

1,3,2-Dioxaphospholane, 2-(2,2,2-trifluoroethoxy)-, 2-oxide synthesis

3synthesis methods
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Yield: 83%

Reaction Conditions:

with Hexamethyldisiloxane;trichlorophosphate at 80 - 90; for 6 h;

Steps:

1-2
A. Mixed reaction: 150 grams of phosphorus oxychloride and 190.5 grams of hexamethyldisiloxane are mixed and reacted for 1 hour; B. Catalyst addition: Add 6 grams of catalyst γ-alumina nanofibers to the reaction solution in step A; C. Dropping reaction: a mixed solution of 66.8 grams of ethylene glycol and 117.4 grams of trifluoroethanol is added dropwise to the reaction solution in step B, and the temperature of the dropping process is controlled at 80°C to 90°C, and the reaction is kept for 5 hours after the addition is completed; D. Vacuum distillation: Collect the fraction from 100°C to 120°C/(10-15) mmHg to obtain 165.3 grams of vinyl trifluoroethyl phosphate, with a yield of 83% and a content of 98.6%.

References:

Jiangsu Huasheng Li Dian Materials Co., Ltd.;Wu Guodong;Lu Haiyuan;Cao Na;Zhou Lixin CN111808137, 2020, A Location in patent:Paragraph 0035-0046