Phosphorus pentachloride → HCID 22761229, compound

HRID 1703438Notes

Reaction equation

HRID 1703438 reaction equation
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([C:6]([NH:8][CH:9](O)[C:10](=[O:15])[C:11]([CH3:14])([CH3:13])[CH3:12])=[O:7])=[CH:4][CH:3]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:20]>C(Cl)(Cl)(Cl)Cl>[Cl:20][CH:9]([NH:8][C:6](=[O:7])[C:5]1[CH:17]=[CH:18][C:2]([Cl:1])=[CH:3][CH:4]=1)[C:10](=[O:15])[C:11]([CH3:14])([CH3:13])[CH3:12]

Participants

4

Procedure

12.1 g (0.05 mol) of 1-(p-chlorobenzamido)-3,3-dimethyl-1-hydroxy-butan-2-one were dissolved in 80 ml. of carbon tetrachloride. 10.4 g (0.05 mol) of phosphorus pentachloride were added at 50° C. and the mixture was then heated for 2 hours under reflux. It was then filtered hot and the filtrate was concentrated in a waterpump vacuum. The crude 1-chloro-1-(p-chlorobenzamido)-3,3-dimethyl-butan-2-one thus obtained could be directly reacted further. The melting point was 132°-135° C. ##STR45##

Workup

  1. temperaturethe mixture was then heated for 2 hours
  2. temperatureunder reflux
  3. filtrationIt was then filtered hot
  4. concentrationthe filtrate was concentrated in a waterpump vacuum

Sources & evidence

ORD record
ord-27ad87d4a71d494484a60fa177a9710f
Source dataset
uspto-grants-1978_11
Patent number
US04124369

Reaction notes

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