HRID323282

反应详情

EQUATION

反应方程式

HRID 323282 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 1-(3,4,5-trimethoxybenzyl)-3-(3-(4-(1-(2-ethoxyethyl)-1H-benzimidazol-2-yl-amino)piperidin-1-yl)propyl)-3-(4-fluorophenylmethyl)-2-oxopyrrolidine (0.91 g, 1.28 mmol) and ethyl acetate (15 mL). Add methanesulfonic acid (0.25 g, 2.57 mmol) and heat to reflux. After 1 hour, cool to ambient temperature and stir. After 12 hours, add diethyl ether and decant the solvent. Repeatedly, add diethyl ether and decant to give a solid. Collect the solid by filtration and dry in vacuo to give the title compound. Rf=0.24 (silica gel, 10% methanol/ethyl acetate/2% triethylamine).

WORKUP

后处理

  1. waitAfter 12 hours
  2. customdecant the solvent
  3. additionRepeatedly, add diethyl ether
  4. customdecant
  5. customto give a solid
  6. customCollect the solid
  7. filtrationby filtration
  8. customdry in vacuo