HRID509479

反应详情

EQUATION

反应方程式

HRID 509479 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 5-(tert-butoxycarbonylamino-methyl)-2-nitro-benzoic acid (21.0 g, 70.9 mmol) in methanol (210 mL) and palladium/carbon (2 g) was hydrogenated with a Parr-shaker overnight at 51 psi. The black mixture was filtered through a pad of Celite, and the filtrate was evaporated to give a brown oil, which was stirred in ether (300 mL) overnight. The ether slurry was filtered to give 2-amino-5-(tert-butoxycarbonylamino-methyl)-benzoic acid as a brown solid (9.3 g, 49% yield). The product was used in the next step without further purification.

WORKUP

后处理

  1. customwas hydrogenated with a Parr-shaker overnight at 51 psi
  2. filtrationThe black mixture was filtered through a pad of Celite
  3. customthe filtrate was evaporated
  4. customto give a brown oil, which
  5. filtrationThe ether slurry was filtered