HRID1430786

反应详情

EQUATION

反应方程式

HRID 1430786 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 3-(bis(tert-butoxycarbonyl)amino)-5-bromo-4-chlorobenzoate (3.06 g, 6.58 mmol) was dissolved in a solution of TFA (1.015 ml, 13.17 mmol) in CH2Cl2 (32.9 ml). The reaction was stirred at rt for 45 min, and then sat. NaHCO3 solution was added. The reaction mixture was diluted with a little more CH2Cl2 and washed 2× with sat. NaHCO3 to remove any residual TFA. The organic layer was dried over Na2SO4, filtered, and concentrated to provide methyl 3-bromo-5-(tert-butoxycarbonylamino)-4-chlorobenzoate (2.33 g) as a cream solid.

WORKUP

后处理

  1. washwashed 2× with sat. NaHCO3
  2. customto remove any residual TFA
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated