HRID440282

反应详情

EQUATION

反应方程式

HRID 440282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customThe crystals formed
  2. filtrationwere filtered
  3. washwashed with 5×10 ml of anhydrous ethanol
  4. customdried
  5. customyielding 9.2 g of raw product, m.p. 252°-254° C. (decomp.)
  6. temperatureAfter cooling the crystals
  7. filtrationwere filtered
  8. washwashed with 3×10 ml of ethanol
  9. customdried