HRID1900061

反应详情

EQUATION

反应方程式

HRID 1900061 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.5 g of (RS)-3-[4-(trans-4-hydroxy-cyclohexyl)-phenyl]-5-methoxymethyl-oxazolidin-2-one in 5 ml of ethyldiisopropylamine was heated with 0.35 ml of chlorodiphenylmethane to 100° and stirred at this temperature for 7 hours. The reaction mixture was cooled, acidified with 1N hydrochloric acid and extracted with ethyl acetate. The organic phase was washed neutral with water, dried with magnesium sulfate and concentrated. The residue (0.7 g) was chromatographed on a 30-fold amount of silica gel with methylene chloride/ethyl acetate mixtures. 0.3 g of (RS)-3-[4-(trans-4-benzhydryloxy-cyclohexyl)-phenyl]-5-methoxymethyl-oxazolidin-2-one was obtained as colorless crystals. M.p.: 146°-148°.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. extractionextracted with ethyl acetate
  3. washThe organic phase was washed neutral with water
  4. dry with materialdried with magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue (0.7 g) was chromatographed on a 30-fold amount of silica gel with methylene chloride/ethyl acetate mixtures