HRID990040

反应详情

EQUATION

反应方程式

HRID 990040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

N-(3,4-Dimethyl-5-isoxazolyl)-5-bromothiophene-2-sulfonamide (680 mg, 2 mmol) in dry THF (2 mL) was added to sodium hydride (121 mg of a 60% oil dispersion, 3 mmol) in dry THF (1 mL). The resulting suspension was cooled to 0° C. and methoxyethoxymethyl chloride (334 mg, 2.68 mmol) was added dropwise via syringe. The solution was warmed to room temperature, and stirring continued overnight. Evaporation of solvent left an oil that was extracted into ethyl acetate, washed with brine, dried over magnesium sulfate and evaporated. Flash chromatography of the residue on silica gel using 10-15% ethyl acetate/hexanes yielded 480 mg (56%) of a colorless oil.

WORKUP

后处理

  1. temperatureThe solution was warmed to room temperature
  2. customEvaporation of solvent
  3. waitleft an oil that
  4. extractionwas extracted into ethyl acetate
  5. washwashed with brine
  6. dry with materialdried over magnesium sulfate
  7. customevaporated