HRID1248433

反应详情

EQUATION

反应方程式

HRID 1248433 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To a stirred mixture of benzylamine (9 ml) and triethylamine (5.5 ml) was added 4-methyl-4-nitro-1-tosyloxypentane (11.9 gm). The mixture was then heated to 70° C. for 2 hrs. The mixture was cooled and partitioned between ethyl acetate and water, the ethyl acetate solution was washed twice with water, then with brine and dried over magnesium sulphate. The solution was evaporated and the product isolated by column chromatography of the residue using gradient elution (Kieselgel; 1:1 60/80 petroleum ether:ethyl acetate going to ethyl acetate). Yield 6.89 gm.

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. custompartitioned between ethyl acetate and water
  3. washthe ethyl acetate solution was washed twice with water
  4. dry with materialwith brine and dried over magnesium sulphate
  5. customThe solution was evaporated
  6. customthe product isolated by column chromatography of the residue
  7. washelution (Kieselgel; 1:1 60/80 petroleum ether:ethyl acetate going to ethyl acetate)