HRID1455401

反应详情

EQUATION

反应方程式

HRID 1455401 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThis solution was warmed to rt over 1 h
  2. temperaturewas cooled to 0° C.
  3. customthe reaction was quenched with Et2O and 1N NaOH
  4. washwashed with saturated Na2S2O3 and NaHCO3 solutions
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated