HRID59584

反应详情

EQUATION

反应方程式

HRID 59584 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

2-Bromo-1-isopropyl-4-nitrobenzene (XI) (20 g, 78.1 mmol, 95.8 GC % by area), methanol (400 ml), platinum on carbon (5% of platinum, poisoned with sulphur, moist with water) (1.0 g, 0.090 mmol) and zinc dibromide (265 mg, 1.18 mmol) were placed in a 600 ml autoclave. The autoclave was subsequently flushed with nitrogen and pressurized to 5 bar with hydrogen at room temperature. The contents of the autoclave were filtered through Celite, washed with methanol and the solvent was distilled off under reduced pressure. 3-Bromo-4-isopropylaniline (17.4 g, 94.5 LC-% by area, 97.7 GC-% by area, >99% of theory) was obtained as a brown oil.

WORKUP

后处理

  1. customThe autoclave was subsequently flushed with nitrogen
  2. custompressurized to 5 bar with hydrogen at room temperature
  3. filtrationThe contents of the autoclave were filtered through Celite
  4. washwashed with methanol
  5. distillationthe solvent was distilled off under reduced pressure