反应详情

A mixture of 1,2-dibenzoyl-5-phenyl-1H-1,2,5-triazepine (25.0 g), dioxane (500 ml), N-hydrochloric acid (250 ml) and 10% Palladium on carbon (1.3 g) was hydrogenated in a Parr apparatus at 16 p.s.i. pressure for 191/2 hours. The catalyst was removed by filtration and washed with water. The filtrate and washings were evaporated to a solid hydrochloride salt which was dried under oil pump vacuum; wt. 22.4 g. The material was assayed by HPLC and shown to be 91% pure. Material prepared in this way was used directly in further syntheses, e.g., in example 8.

1. custom2 hours
2. customThe catalyst was removed by filtration
3. washwashed with water
4. customThe filtrate and washings were evaporated to a solid hydrochloride salt which
5. customwas dried under oil pump vacuum
6. customMaterial prepared in this way