HRID2387282

反应详情

EQUATION

反应方程式

HRID 2387282 反应方程式

PROCEDURE

实验过程

To sodium hydride (0.174 g, 4.35 mmol) in tetrahydrofuran (6.8 mL, 0.084 mol), 1H-Indole-6-carbaldehyde (59, 0.486 g, 3.35 mol) was added. After 30 minutes, propane-1-sulfonyl chloride (0.565 mL, 5.02 mol) was added. After two hours, it was quenched with 1M HCl (aqueous) and extracted twice with ethyl acetate. The combined organic layers were washed with brine, dried over anhydrous sodium sulfate and filtered. The filtrate was concentrated. The desired compound was purified by silica gel column chromatography eluting with a gradient of ethyl acetate in hexane to give 516 mg of desired compound. MS (ESI) [M−H+]−=250.1.

WORKUP

后处理

  1. waitAfter two hours
  2. customit was quenched with 1M HCl (aqueous)
  3. extractionextracted twice with ethyl acetate
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated
  8. customThe desired compound was purified by silica gel column chromatography
  9. washeluting with a gradient of ethyl acetate in hexane