HRID2303679

反应详情

EQUATION

反应方程式

HRID 2303679 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (+−)-trans-3-hydroxymethyl-4-phenylcyclopentan-1-one from Step C (5.0 g, 24 mmol) in methylene chloride (100 mL) was added t-butyldimethylsilyl chloride (11.5 g, 48 mmol) and DIPEA (8.6 mL, 48 mmol). The reaction mixture was stirred at rt for 16 h, poured into dilute aq. HCl and extracted twice with ether. The organic layers were washed with brine, dried over sodium sulfate, combined and concentrated. The residue was purified by FC (5% ethyl acetate in hexanes) to afford the title compound (6.5 g) as a oil.

WORKUP

后处理

  1. extractionextracted twice with ether
  2. washThe organic layers were washed with brine
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by FC (5% ethyl acetate in hexanes)