HCID 12639764, compound → HCID 12639769, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 3,750 ml of hydrochloric acid, 134 g of 2-methyl-3-nitro-4'-chloro-benzophenone and 536 g of stannous chloride was heated at 62° C for 6 hours and was then cooled to 5° C and held therefor 1 hour. The mixture was vacuum filtered and the precipitate was washed with hydrochloric acid and dried under reduced pressure. The residue was stirred for 2 hours at room temperature with 1,300 ml of water, 1,000 ml of 2N sodium hydroxide and 230 ml of ether and the mixture was then extracted with methylene chloride. The organic phase was washed with water, dried over sodium sulfate and evaporated to dryness under reduced pressure to obtain 68.7 g of 2-methyl-3-amino-4'-chloro-benzophenone melting at 65° C which was used as is for the next step.

Provenance & Evidence