反应详情

1 g of 4-(3-tert-butylamino-2-hydroxypropoxy)oxindole, 20 cc of chloroform, 10 cc of pyridine and 0.713 g of nicotinoyl chloride are allowed to stand at room temperature for 4 days, the mixture is then concentrated by evaporation as carefully as possible at reduced pressure and the residue is taken up in water. The reaction mixture is rendered alkaline with a 10% ammonia solution, is extracted with methylene chloride, and subsequently an excess of 2 N hydrochloric acid in ethanol is added. The solvent and excess hydrochloric acid are carefully removed by evaporation at reduced pressure and the dihydrochloride of the title compound is crystallized from ethanol, needle druses. M.P. 215°-218° .

1. concentrationthe mixture is then concentrated by evaporation as carefully as possible at reduced pressure
2. extractionis extracted with methylene chloride
3. additionsubsequently an excess of 2 N hydrochloric acid in ethanol is added
4. customThe solvent and excess hydrochloric acid are carefully removed by evaporation at reduced pressure
5. customthe dihydrochloride of the title compound is crystallized from ethanol, needle druses