HRID1502620

反应详情

EQUATION

反应方程式

HRID 1502620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium t-butoxide (3.3 g, 29.4 mmol) was added to a mixture of ketone (3, 2.5 g, 18.1 mmol) and trimethylsulfoxonium iodide (6.45 g, 29.4 mmol) in dry dimethyl sulfoxide (40 mL) under nitrogen atmosphere at room temperature. The mixture was stirred for 4.0 h at room temperature. The reaction was quenched by the addition of cold water (40 mL) and extracted with ethyl acetate (2×60 mL). The combined organic layer was washed with water (75 mL) followed by brine (75 mL) and dried over sodium sulfate. The filtered organic layer was concentrated under vacuum to give an oil. Weight: 2.13 g. Weight yield: 77%. 1H-NMR (400 MHz, CDCl3): δ 1.42-1.50 (m, 2H), 1.55-1.61 (m, 2H), 1.65 (s, 6H), 2.31 (t, 4H), 2.61 (s, 2H). MS (APCI method): No molecular ion peak was observed.

WORKUP

后处理

  1. customThe reaction was quenched by the addition of cold water (40 mL)
  2. extractionextracted with ethyl acetate (2×60 mL)
  3. washThe combined organic layer was washed with water (75 mL)
  4. dry with materialdried over sodium sulfate
  5. concentrationThe filtered organic layer was concentrated under vacuum
  6. customto give an oil