HRID238896

反应详情

EQUATION

反应方程式

HRID 238896 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.0 g 5,6,7,8-tetrahydro-naphthalen-1-ol was dissolved in 20 ml of N,N-dimethylformamide. To this solution was added slowly 0.256 g of 95% NaH, followed by addition of 0.768 ml of chloromethoxymethane. The reaction was flushed with nitrogen and left stirring overnight at room temperature. The reaction mixture was then diluted with 50 ml of water and extracted with 50 ml of diethyl ether. The organic layer was washed with 50 ml of water, dried over magnesium sulphate and concentrated in vacuo to afford a crude oil. This was purified by flash chromatography (silica, heptanes/dichloro-methane) to afford 1.0 g of 5-methoxymethoxy-1,2,3,4-tetrahydro-naphthalene.

WORKUP

后处理

  1. customThe reaction was flushed with nitrogen
  2. waitleft
  3. additionThe reaction mixture was then diluted with 50 ml of water
  4. extractionextracted with 50 ml of diethyl ether
  5. washThe organic layer was washed with 50 ml of water
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated in vacuo
  8. customto afford a crude oil
  9. customThis was purified by flash chromatography (silica, heptanes/dichloro-methane)