HRID1786481

反应详情

EQUATION

反应方程式

HRID 1786481 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of [5-(1-isopropyl-piperidin-4-yloxy)-1H-indol-2-yl]-piperazin-1-yl-methanone dihydrochloride (82 mg, 0.22 mmol) in dichloromethane (2 ml) were added triethylamine (4.2 eq, 0.13 ml) and methanesulfonyl chloride (1.4 eq, 0.02 ml). The mixture was stirred overnight, diluted with dichloromethane and washed with 1N aqueous sodium bicarbonate solution. The phases were separated, the aqueous phase extracted with dichloromethane, and the combined organic phases washed with brine and dried over magnesium sulfate. The crude product was purified by column chromatography on silica gel (1:0 to 5:1 dichloromethane/methanol eluant) to afford the title compound as an off-white solid. MS (m/z): 449.2 (M+H)+.

WORKUP

后处理

  1. washwashed with 1N aqueous sodium bicarbonate solution
  2. customThe phases were separated
  3. extractionthe aqueous phase extracted with dichloromethane
  4. washthe combined organic phases washed with brine
  5. dry with materialdried over magnesium sulfate
  6. customThe crude product was purified by column chromatography on silica gel (1:0 to 5:1 dichloromethane/methanol eluant)