HRID2171739

反应详情

EQUATION

反应方程式

HRID 2171739 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

To a mixture of (R)-epichlorohydrin (2.2 g, 23.8 mmol) and 5,5-dimethyl-5,6,7,8-tetrahydro-naphthalen-2-ol (2.1 g, 11.9 mmol) in acetone (30 ml) was added potassium carbonate (1.65 g, 11.9 mmol). The mixture was stirred at 45° C. for 7 days. The reaction mixture was then concentrated. The residue was partitioned between ethyl acetate and water and extracted twice with ethyl acetate. The organic extracts were combined and washed with water, brine, dried over sodium sulfate and concentrated under vacuum. The resulting residue was purified by flash chromatography (silica, methylene chloride/heptane) to give 1.84 g (67%) of (S)-2-(5,5-dimethyl-5,6,7,8-tetrahydro-naphthalen-2-yloxymethyl)-oxirane.

WORKUP

后处理

  1. concentrationThe reaction mixture was then concentrated
  2. customThe residue was partitioned between ethyl acetate and water
  3. extractionextracted twice with ethyl acetate
  4. washwashed with water, brine
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated under vacuum
  7. customThe resulting residue was purified by flash chromatography (silica, methylene chloride/heptane)