HRID1819454

反应详情

EQUATION

反应方程式

HRID 1819454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[4-({5-Nitro-2-[(quinolin-5-ylmethyl)-amino]-pyrimidin-4-ylamino}-methyl)-cyclohexyl]-carbamic acid tert-butyl ester (197 mg, 0.39 mmol) was dissolved in CH2Cl2 (10 mL) and TFA (2 mL) was added. The reaction mixture was stirred at room temperature for 1 h. The reaction mixture was treated with 3M Na2CO3 and the organic phase was separated. The organic phase was dried over Na2SO4 and concentrated. Silica gel purification using a mixture of 10:1:0.3 CH2Cl2:MeOH:Et3N yielded 120 mg of the title compound as a light yellow solid (79%), m/z 406.4 [M−1]+.

WORKUP

后处理

  1. customthe organic phase was separated
  2. dry with materialThe organic phase was dried over Na2SO4
  3. concentrationconcentrated
  4. customSilica gel purification
  5. additiona mixture of 10:1:0.3 CH2Cl2