methyl ([(benzyloxy)carbonyl]amino)-(dimethoxyphosphoryl)acetate synthesis
- Product Name:methyl ([(benzyloxy)carbonyl]amino)-(dimethoxyphosphoryl)acetate
- CAS Number:100945-15-1
- Molecular formula:C13H18NO9P
- Molecular Weight:363.2571
Yield:100945-15-1 90%
Reaction Conditions:
Stage #1: methyl 2-(benzyloxycarbonylamino)-2-methoxyacetatewith phosphorus trichloride in toluene at 70; for 12 h;
Stage #2: phosphorous acid trimethyl ester in toluene at 70; for 4 h;
Steps:
1.c
c) Compound 4 (118.6mmol, 1.0eq) andPhosphorus trichloride (130.5mmol, 1.1eq)Dissolved in 250mL toluene,The reaction solution was reacted at 70°C for 12h,TLC detection found that compound 4 disappeared,It is transformed into a chlorinated product with greater polarity than compound 4.The reaction solution was cooled to room temperature, trimethyl phosphite (130.5mmol, 1.1eq) was slowly added, and the reaction solution was reacted at 70°C for 4h,TLC detects complete conversion of the chlorinated product, and product 5 is obtained.Post-treatment: at 45-50, remove the solvent toluene and volatile matter by rotary evaporation,The concentrated solution was slowly poured into saturated sodium bicarbonate, extracted with ethyl acetate, dried over magnesium sulfate, and concentrated.Isopropyl ether was added to the concentrate and stirred to obtain 35.3 g of white solid compound 5 with a yield of 90%.
References:
CN113185549,2021,A Location in patent:Paragraph 0030-0032; 0038-0040
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