HRID1374305
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
Benzyl (S)-1-((1S,2S,4R)-4-hydroxy-2-isopropylcyclohexyl)-2-oxopyrrolidin-3-ylcarbamate (333 mg) was dissolved in CH2Cl2 (5 mL) and cooled to 0° C. prior to the addition of Dess-Martin reagent (678.9 mg). This solution was warmed to rt over 1 h, and then was cooled to 0° C. prior to the addition of more Dess-Martin reagent (260 mg). After 1 h at rt, the reaction was quenched with Et2O and 1N NaOH. The organic extracts were combined, washed with saturated Na2S2O3 and NaHCO3 solutions, dried (MgSO4), filtered, and concentrated to afford benzyl (S)-1-((1S,2S)-2-isopropyl-4-oxocyclohexyl)-2-oxopyrrolidin-3-ylcarbamate (350 mg). MS found: (M+H)+=373.4.
WORKUP
后处理
- temperatureThis solution was warmed to rt over 1 h
- temperaturewas cooled to 0° C.
- customthe reaction was quenched with Et2O and 1N NaOH
- washwashed with saturated Na2S2O3 and NaHCO3 solutions
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated