Acetyl chloride → 1-Acetyl-2-Diethoxyphosphoryl Hydrazine

Diethylphosphorohydrazidate (5.3 g) and triethylamine (13 ml) were dissolved in dichloromethane (15 ml). To this solution was added dropwise with stirring and cooling a solution of acetyl chloride (7.4 g) in dichloromethane (15 ml). The mixture was then stirred at ambient temperature and then filtered to remove the triethylamine hydrochloride after the addition of 50 ml of anhydrous diethylether. The filtrates were stripped on a rotary evaporator to yield a red-brown oil which was distilled under high vacuum to give a pale yellow liquid, b.p. 180° C./1 mm, identified as the product.

1. additionTo this solution was added dropwise
2. stirringThe mixture was then stirred at ambient temperature
3. filtrationfiltered
4. customto remove the triethylamine hydrochloride
5. additionafter the addition of 50 ml of anhydrous diethylether
6. customThe filtrates were stripped on a rotary evaporator
7. customto yield a red-brown oil which
8. distillationwas distilled under high vacuum
9. customto give a pale yellow liquid, b.p. 180° C./1 mm

ORD record

ord-e7333ed741b948dc9645cae461eecfb7

Source dataset

uspto-grants-1980_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04203932