Water → HCID 86720047, compound

Participants

Reaction Conditions

Reaction Steps

109.00 g (249.95 mmol) of the compound from example 78A were initially charged in sulfolane (490 ml), then 55.92 ml (599.88 mmol) of phosphoryl chloride were added and the mixture was heated to 120° C. for 1 h. After cooling, the mixture was added cautiously to water (3 l) and stirred for 15 min. Sodium hydrogencarbonate was added in portions until the pH was 6. The precipitate formed was filtered off with suction and washed with water. The residue was stirred with 200 ml of dichloromethane/methanol (v/v=4:1) for 30 min, filtered off with suction, washed with dichloromethane, acetone and petroleum ether and dried under high vacuum. This gave 63.00 g (62% of theory) of the title compound.

Provenance & Evidence