HRID216408

反应详情

EQUATION

反应方程式

HRID 216408 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

Step C, 1.5 N Hydrochloric acid (1 mL) was added to a solution of 4-(2,2-dimethylpropyl)-2-{hydroxy[2-(4-pyridin-2-ylphenyl)-1,3-dithian-2-yl]methyl}-N,N-dimethyl-1H-imidazole-1-sulfonamide in tetrahydrofuran (1 mL). After heating in a sealed tube at 70° C. for a few minutes until no further reaction (LCMS), the reaction mixture was cooled to 0° C., quenched with 10% aqueous sodium hydroxide and extracted with ethyl acetate. The combined organic extracts were dried (magnesium sulfate) and concentrated in vacuo. Preparatory plate chromatography eluting with 10% methanol/ethyl aceate afforded the title compound. LCMS: 440 (M+H).

WORKUP

后处理

  1. temperaturethe reaction mixture was cooled to 0° C.
  2. customquenched with 10% aqueous sodium hydroxide
  3. extractionextracted with ethyl acetate
  4. dry with materialThe combined organic extracts were dried (magnesium sulfate)
  5. concentrationconcentrated in vacuo
  6. washPreparatory plate chromatography eluting with 10% methanol/ethyl aceate