HRID2196700

反应详情

EQUATION

反应方程式

HRID 2196700 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Cyclopropyl(1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridin-3-yl)methanol (0.285 g, 0.87 mmol) was dissolved in dry dichloromethane (9 mL) and chilled to 0° C. Triethylsilane (1.11 mL, 6.94 mmol, 8 eq.) and TFA (0.201 mL, 2.60 mmol, 3 eq.) were then added. The reaction mixture was stirred at 0° C. for 15 minutes and then allowed to warm to room temperature. After about 1.5 hours, the mixture was quenched with saturated sodium bicarbonate solution and extracted with DCM. The extracts were dried over sodium sulfate and concentrated. Flash 40 Biotage (40M cartridge, DCM to 5% EtOAc/DCM) afforded 3-(cyclopropylmethyl)-1-(phenylsulfonyl)-1H-pyrrolo[2,3-b]pyridine (159 mg, 59%). m/z (APCI-pos) M+1=313.1.

WORKUP

后处理

  1. temperatureto warm to room temperature
  2. waitAfter about 1.5 hours
  3. customthe mixture was quenched with saturated sodium bicarbonate solution
  4. extractionextracted with DCM
  5. dry with materialThe extracts were dried over sodium sulfate
  6. concentrationconcentrated