HRID261987

反应详情

EQUATION

反应方程式

HRID 261987 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6.86 g of the anti isomer of ethyl 2-(2-tritylamino-4-thiazolyl)-2-hydroxyiminoacetate of Example 14, 3.51 g of potassium carbonate in 15 ml of dimethylformamide and 7.7 ml of isopropyl iodide was held under an argon atmosphere and stirring for 41/2 hours and then 250 ml of distilled water and 150 ml of ethyl acetate were added thereto with stirring. The mixture was decanted and the aqueous phase was washed with water and was extracted with ethyl acetate. The organic phase was dried, vacuum filtered and evaporated to dryness. The residue was taken up in ethanol and crystallization stated after seeding. The mixture was vacuum filtered and the precipitate was rinsed with ethanol and empasted with petroleum ether to obtain 3.26 g of the anti isomer of ethyl 2-(2-tritylamino-4-thiazolyl)-2-(1-methylethoxyimino)-acetate melting at 182° C.

WORKUP

后处理

  1. stirringwith stirring
  2. customThe mixture was decanted
  3. washthe aqueous phase was washed with water
  4. extractionwas extracted with ethyl acetate
  5. customThe organic phase was dried
  6. filtrationvacuum filtered
  7. customevaporated to dryness
  8. customcrystallization
  9. filtrationfiltered
  10. washthe precipitate was rinsed with ethanol