HRID2059942

反应详情

EQUATION

反应方程式

HRID 2059942 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 2-[(1-methylethyl)oxy]-5-[3-(5-methyl-1,2,3,4-tetrahydro-6-isoquinolinyl)-1,2,4-oxadiazol-5-yl]benzonitrile trifluoroacetic acid salt (Example 11; 100 mg, 0.20 mmol), ethyl bromoacetate (44 mg, 30 μl, 0.26 mmol) and caesium carbonate (200 mg, 0.61 mmol) in dry DMF (3 ml) was stirred at room temperature for 1 hour. The reaction mixture was diluted with water (10 ml) and extracted with ethyl acetate (3×5 ml). The combined extracts were dried and evaporated. Purification by chromatography on silica gel, eluting with 10% ethyl acetate in cyclohexane gave the title compound as a colourless oil (85 mg). MS m/z 461 [MH]+.

WORKUP

后处理

  1. extractionextracted with ethyl acetate (3×5 ml)
  2. customThe combined extracts were dried
  3. customevaporated
  4. customPurification by chromatography on silica gel
  5. washeluting with 10% ethyl acetate in cyclohexane