HRID2235317
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureReflux for 2 hours
- concentrationconcentrate under vacuum
- custompurify by chromatography
- customto recover 145 mg (36%) of a foam
- customHPLC (5 to 95) Rt (Purity at 214 nm)=4.703 min (99%)