HRID2275036

反应详情

EQUATION

反应方程式

HRID 2275036 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of (R)-tert-butyl(1-(2-(1-ethyl-1H-pyrrolo[2,3-c]pyridin-2-yl)-1-methyl-1H-benzo[d]imidazole-5-carbonyl)piperidin-3-yl)carbamate (42 mg, 0.084 mmol) in dichloromethane (DCM) (1 mL) was added TFA (0.258 mL, 3.34 mmol) and the reaction stirred at room temperature for 2 h. The reaction mixture was concentrated in vacuo to afford a yellow oil. This was dissolved in methanol and loaded onto an SCX cartridge (5 g). It was eluted with methanol (3 column volumes) and product eluted as free base with 2M ammonia in methanol. The filtrate from the ammonia fractions was concentrated in vacuo to yield the title compound as a yellow solid (34 mg).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customto afford a yellow oil
  3. washIt was eluted with methanol (3 column volumes) and product
  4. washeluted as free base with 2M ammonia in methanol
  5. concentrationThe filtrate from the ammonia fractions was concentrated in vacuo