HRID1900069

反应详情

EQUATION

反应方程式

HRID 1900069 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

932 mg (2.6 mmol) of (R)-3-[trans-4-[4-(5-methoxymethyl-2-oxo-oxazolidin-3-yl)-phenyl]-cyclohexyloxy]-propionitrile were dissolved in 60 ml of methanol saturated with dry ammonia gas and hydrogenated in the presence of 0.9 g of Raney-nickel (Type B 113W Degussa). After 3 hours the catalyst was filtered off under suction and the filtrate was evaporated. The residue was dissolved in methylene chloride, washed with water, dried over sodium sulfate, filtered and evaporated. The base was dissolved in alcohol and made acid with ethereal hydrochloric acid. After recrystallization from alcohol-ether there were obtained 825.2 mg of (R)-3-[trans-4-(3-amino-propoxy)-cyclohexyl]-phenyl]-5-methoxymethyl-oxazolidin-2-one.HCl. M.p.: 178°-180°. [α]D =-29.78° (c=1% in CHCl3).

WORKUP

后处理

  1. filtrationAfter 3 hours the catalyst was filtered off under suction
  2. customthe filtrate was evaporated
  3. dissolutionThe residue was dissolved in methylene chloride
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customevaporated
  8. dissolutionThe base was dissolved in alcohol
  9. customAfter recrystallization from alcohol-ether