HRID1248432

反应详情

EQUATION

反应方程式

HRID 1248432 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-methyl-4-nitro-1-pentanol (7 gm) in pyridine (40 ml) was cooled in an ice bath and treated with tosyl chloride (19 gm) added in portions over 20 mins. When the addition was complete the mixture was stirred at room temperature for 1 hr. Water (20 ml) was then added and the mixture stirred for 15 mins. The mixture was poured into water and extracted twice with ethyl acetate. The ethyl acetate solution was washed successively with water, citric acid solution, water, sodium bicarbonate solution, water and brine. The solution was dried over magnesium sulphate and evaporated. The product was obtained by crystallisation from ether: 60/80 petroleum ether. Yield 8.18 gm.

WORKUP

后处理

  1. additionadded in portions over 20 mins
  2. additionWhen the addition
  3. stirringthe mixture stirred for 15 mins
  4. extractionextracted twice with ethyl acetate
  5. washThe ethyl acetate solution was washed successively with water, citric acid solution, water, sodium bicarbonate solution, water and brine
  6. dry with materialThe solution was dried over magnesium sulphate
  7. customevaporated
  8. customThe product was obtained by crystallisation from ether