HRID616273

反应详情

EQUATION

反应方程式

HRID 616273 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 17.3 g (0.053 mol) of the compound of Example 40 and 6.3 g (0.53 mol) of methyl nitroacetate in 115 ml of acetic anhydride was heated at 95° for 1 hour. The mixture was concentrated, the residue slurried with ether, filtered and washed with ether to give 17.6 g (78%) of red orange crystals, m.p. 158°-165°. Recrystallization from benzene-dimethylformamide afforded 13.4 g (59%) of product, m.p. 179°-181°.

WORKUP

后处理

  1. temperaturewas heated at 95° for 1 hour
  2. concentrationThe mixture was concentrated
  3. filtrationfiltered
  4. washwashed with ether