HRID1981100

反应详情

EQUATION

反应方程式

HRID 1981100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

30 parts of 9-hydroxy-3,4-diazatricyclo[4,2,1,02,5 ]-nona-3,7-diene and 34 parts of p-chlorophenyl azide in 100 parts of toluene were heated at 80° C. for 3 hours, while stirring. The mixture was evaporated down in a rotary evaporator at from 20° to 40° C. and under 20 mbar, after which the residue was digested successively with 100 parts of diethyl ether and 100 parts of petroleum ether, and the product was dried at 20° C. under 1 mbar. 59 parts (92 mole %) of 8-(4-chlorophenyl)-12-hydroxy-3,4,8,9,10-pentazatetracyclo[5,4,1,02,5,07,11 ]dodeca-3,9-diene of melting point 178° C. (decomposition) were obtained (Command No. 1). ##STR20##

WORKUP

后处理

  1. customThe mixture was evaporated down in a rotary evaporator at from 20° to 40° C. and under 20 mbar
  2. customthe product was dried at 20° C. under 1 mbar