HRID440282
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
10 g (34 mmol) of 1-(4-aminophenyl)-4-methyl-7,8-methylenedioxy-5H-2,3-benzodiazepine were stirred for 3 hours with 100 ml of acetic anhydride. The crystals formed were filtered, washed with 5×10 ml of anhydrous ethanol and dried, yielding 9.2 g of raw product, m.p. 252°-254° C. (decomp.). This product was treated with 45 ml of hot 99.5% ethanol. After cooling the crystals were filtered, washed with 3×10 ml of ethanol and dried to give 8.68 g (76.1%) of the aimed product, m.p.: 256°-258° C. (decomp.).
WORKUP
后处理
- customThe crystals formed
- filtrationwere filtered
- washwashed with 5×10 ml of anhydrous ethanol
- customdried
- customyielding 9.2 g of raw product, m.p. 252°-254° C. (decomp.)
- temperatureAfter cooling the crystals
- filtrationwere filtered
- washwashed with 3×10 ml of ethanol
- customdried