HRID1358979

反应详情

EQUATION

反应方程式

HRID 1358979 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

Stannous chloride (0.182 g, 0.0096 mole) was added to the suspension of 2-isopropylcarbonylamino-6-acetamido-3-(2,3,5-trichlorophenyl)pyrazine (0.13 g, 3.24×10−4 mole), in absolute ethanol (6.50 ml) and the resulting mixture stirred at 50-60° C. for 1 hr 20 min. The reaction mixture was cooled and evaporated in vacuo. The residue was extracted with ethylacetate (3×20 ml), washed with water (2×20 ml), dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated in vacuo. The residue was purified by ‘flash chromatography’ using chloroform:methanol, 99:1 as the eluent. Yield 0.046 g (40%), M.p. 105-108° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. customevaporated in vacuo
  3. extractionThe residue was extracted with ethylacetate (3×20 ml)
  4. washwashed with water (2×20 ml)
  5. dry with materialdried over anhydrous magnesium sulphate
  6. filtrationfiltered
  7. customthe filtrate evaporated in vacuo
  8. customThe residue was purified by ‘flash chromatography’