HRID2235317

反应详情

EQUATION

反应方程式

HRID 2235317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 0.5 g (0.9 mmol) 3-(4-benzyloxy-2,6-dichloro-benzyl)-1-[cis-4-(tert-butyl-dimethyl-silanyloxy)-cyclohexyl]-pyrrolidin-2-one (Preparation 71) with 25 mL THF and treat with 0.5 mL 1 M TBAF in THF. Reflux for 2 hours, concentrate under vacuum and purify by chromatography using a gradient (CHCl3>10% MeOH) to recover 145 mg (36%) of a foam. Mass spectrum (apci) m/z=448 (M+). HPLC (5 to 95) Rt (Purity at 214 nm)=4.703 min (99%).

WORKUP

后处理

  1. temperatureReflux for 2 hours
  2. concentrationconcentrate under vacuum
  3. custompurify by chromatography
  4. customto recover 145 mg (36%) of a foam
  5. customHPLC (5 to 95) Rt (Purity at 214 nm)=4.703 min (99%)