HRID629875

反应详情

EQUATION

反应方程式

HRID 629875 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-(2,2-Dimethylpropyl)-5-(1,2,3,3a,4,6a-hexahydrocyclopenta[c]pyrrol-5-yl)-3-methyl-1,3-dihydro-2H-imidazo[4,5-b]pyridin-2-one (8-4, 100 mg, 0.30 mmol, 1.0 equiv), and DIPEA (0.16 mL, 0.91 mmol, 3.0 equiv) were added to anhydrous methylene chloride (3 mL) Stirred for 5 min and acetyl chloride (26.5 mg, 0.33 mmol, 1.1 equiv) was added. After stirring for 10 min at room temperature, LCMS showed consumption of starting material. Purification by reverse-phase HPLC (20-100% CH3CN:0.1% TFA in H2O) provided 9-1 as a pale yellow oil. MS m/z (M+H): calculated=369.2287; observed=369.2298.

WORKUP

后处理

  1. stirringAfter stirring for 10 min at room temperature
  2. customconsumption of starting material
  3. customPurification by reverse-phase HPLC (20-100% CH3CN:0.1% TFA in H2O)