Phosphorus pentachloride → HCID 22761229, compound
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
Reactant 2
Product 1
Reagents, catalysts & solvents 1
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
- temperaturethe mixture was then heated for 2 hours
- temperatureunder reflux
- filtrationIt was then filtered hot
- 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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