Synthesis method of (R,S)-S-secondary butyl o-ethyl-2-oxo-1,3-thiazolidine-3-thiosulphate
A technology of ethyl thiophosphoryl and synthesis method, applied to (R,S)-S-sec-butyl-O-ethyl-2-oxo-1,3-thiazolidine-3-ylthio In the field of phosphate synthesis, it can solve the problems of affecting product content, complex synthesis process, and low intermediate content, and achieve the effects of simple operation, high yield, and easy availability of raw materials.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0022] In a 500 mL four-neck flask, add 31.2 g (0.3 mol) of 2-thiazolidinone, 42.2 mL (0.3 mol) of triethylamine and 200 mL of toluene, and stir electrically. Heated to 100°C, and 67.5 mL (0.42 mol) of O, O'-diethylthiophosphoryl chloride was added dropwise. After the dropwise addition, the reaction was continued for 4 hours. After the reaction is completed, cool to room temperature, wash with water, dry the toluene layer with anhydrous sodium sulfate, filter, and precipitate to obtain brown-yellow O, O'-diethyl-2-oxo-1,3-thiazolidin-3-yl phosphorothioate.
[0023] In a 250 mL four-necked flask, add the above O, O'-diethyl-2-oxo-1,3-thiazolidin-3-yl phosphorothioate (calculated as 0.276 mol) and 82.5 mL (0.55 mol) of 33 % dimethylamine aqueous solution, stirred, heated to reflux, and incubated for 20 hours. The reaction was stopped, and the reaction solution was concentrated to obtain light yellow viscous phosphorothioate ammonium salt. Add the above-mentioned ammonium pho...
Embodiment 2
[0029] In a 500 mL four-neck flask, add 31.2 g (0.3 mol) of 2-thiazolidinone, 27.2 mL (0.33 mol) of pyridine and 200 mL of toluene, and stir electrically. After heating to 90°C, 57.9 mL (0.36 mol) of O, O'-diethylthiophosphoryl chloride was added dropwise. After the dropwise addition, the reaction was continued for 7 hours. After the reaction is completed, cool to room temperature, wash with water, dry the toluene layer with anhydrous sodium sulfate, filter, and precipitate to obtain brown-yellow O, O'-diethyl-2-oxo-1,3-thiazolidin-3-yl phosphorothioate.
[0030] In a 250mL four-necked flask, add the above-mentioned O, O'-diethyl-2-oxo-1,3-thiazolidin-3-yl phosphorothioate (calculated as 0.273mol) and 182mL (0.82mol) of 33% Diethylamine aqueous solution was stirred, heated to reflux, and kept for 30 hours for reaction. Stop the reaction and concentrate to obtain light yellow viscous phosphorothioate ammonium salt. Add the above-mentioned ammonium phosphorothioate into a 25...
Embodiment 3
[0032] In a 500 mL four-neck flask, add 31.2 g (0.3 mol) of 2-thiazolidinone, 40.3 g (0.33 mol) of 4-dimethylaminopyridine and 200 mL of xylene, and stir electrically. After heating to 90°C, 57.9 mL (0.36 mol) of O, O'-diethylthiophosphoryl chloride was added dropwise. After the dropwise addition, the reaction was continued for 7 hours. After the reaction is completed, cool to room temperature, wash with water, dry the toluene layer with anhydrous sodium sulfate, filter, and precipitate to obtain brown-yellow O, O'-diethyl-2-oxo-1,3-thiazolidin-3-yl phosphorothioate.
[0033] In a 250 mL four-necked flask, add the above O, O'-diethyl-2-oxo-1,3-thiazolidin-3-yl phosphorothioate (calculated as 0.273 mol) and 82.5 mL (0.55 mol) of 33 % dimethylamine aqueous solution, stirred, heated to reflux, and incubated for 30 hours. Stop the reaction and concentrate to obtain light yellow viscous phosphorothioate ammonium salt. Add the above-mentioned ammonium phosphorothioate into a 250...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More