HRID638522

反应详情

EQUATION

反应方程式

HRID 638522 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 18.9 g N-methyl-3-formyl carbazole in 400 ml ethanol, a mixture of 2.5 g NaBH4 and 20 ml 0.4N NaOH in water was added dropwise. The mixture was then heated at 60° C. and stirred for one hour. Cooling at room temperature, white crystals were obtained which were filtered, washed with water, dried and recrystallized from a cyclohexane:benzene mixture (1:1), yielding 92% N-methyl-3-hydroxymethyl carbazole with m.p.=96° C. IR: 3346 cm-1 (OH), 710, 729, 747, 770, 804 cm-1 (carbazole) 1H.NMR (CDCl3): 8.13-8.03 ppm (C4, C5, multiplet) 7.43-7.29 ppm (C1, C2, C6, C7, C8, multiplet) 4.84 ppm (CH2 singlet) 3.83 ppm (CH3 singlet) 1.64 ppm (OH, singlet).

WORKUP

后处理

  1. additionwas added dropwise
  2. temperatureCooling at room temperature
  3. customwhite crystals were obtained which
  4. filtrationwere filtered
  5. washwashed with water
  6. customdried
  7. customrecrystallized from a cyclohexane