HRID1036959

反应详情

EQUATION

反应方程式

HRID 1036959 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Pyridine-3-sulfonyl chloride (96 mg, 0.54 mmol) was added dropwise a mixture of 3-(4,4,6-trimethyl-1,2,3,4-tetrahydro-quinolin-2-yl)-phenylamine (120 mg, 0.45 mmol) and pyridine (60 mg, 0.76 mmol) in dichloromethane (5 mL). The resultant mixture was allowed to stir overnight. The reaction mixture was washed by water, dried over magnesium sulfate. The mixture was filtered and concentrated to provide the crude product. It was purified by column chromatography (silica gel, petroleum ether:ethyl acetate=4:1) to afford pyridine-3-sulfonic acid [3-(4,4,6-trimethyl-1,2,3,4-tetrahydro-quinolin-2-yl)-phenyl]-amide as off-white solid (25 mg, yield: 13.7%). MS (ESI+APCI) M+1=408.2.

WORKUP

后处理

  1. washThe reaction mixture was washed by water
  2. dry with materialdried over magnesium sulfate
  3. filtrationThe mixture was filtered
  4. concentrationconcentrated
  5. customto provide the crude product
  6. customIt was purified by column chromatography (silica gel, petroleum ether:ethyl acetate=4:1)