Formic Acid → HCID 20283629、化合物

A reaction mixture consisting of 2,2-dichloroacetamide (6.4 g, 50 mmol), phosphorus pentachloride (10.4 g, 50 mmol), and carbon tetrachloride (50 mL) was stirred under nitrogen while heated at reflux for 30 minutes. A clear solution resulted, which was cooled to room temperature. Formic acid (1.9 mL, 50 mmol) was added dropwise with stirring, and formation of a white precipitate was observed. The stirring was continued for 1 hour at ambient temperature. The white solid was separated by filtration, rinsed with carbon tetrachloride, and dried in vacuum over phosphorus pentoxide at ambient temperature. A yield of 10 g (82%) of N-(dichlorophosphinyl)-2,2-dichloroacetamide was obtained.

1. temperaturewhile heated
2. temperatureat reflux for 30 minutes
3. customA clear solution resulted
4. stirringwith stirring
5. customThe white solid was separated by filtration
6. washrinsed with carbon tetrachloride
7. dry with materialdried in vacuum over phosphorus pentoxide at ambient temperature

ORDレコード

ord-829e607fdc6d4cdf9a2fffde99dfb037

出典データセット

uspto-grants-1985_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04517003