HRID2238674

反应详情

EQUATION

反应方程式

HRID 2238674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

80 mg of the t-butyl{(1S)-1-[4-(4-methylpiperazin-1-yl)phenyl]ethyl}carbamate [107-1] was dissolved in 3 mL of chloroform, then 70 mg of N-chlorosuccinimide was added thereto, and stirred at room temperature for 2 hours. The reaction solution was diluted with chloroform, washed with a saturated aqueous solution of sodium hydrogen carbonate, and dried over anhydrous magnesium sulfate. The insolubles were filtered, the filtrate was concentrated under reduced pressure, and thus obtained residue was purified by preparative thin-layer chromatography, to obtain 80 mg of t-butyl{(1S)-1-[3-chloro-4-(4-methylpiperazin-1-yl)phenyl]ethyl}carbamate [139-1] as a colorless oily product.

WORKUP

后处理

  1. washwashed with a saturated aqueous solution of sodium hydrogen carbonate
  2. dry with materialdried over anhydrous magnesium sulfate
  3. filtrationThe insolubles were filtered
  4. concentrationthe filtrate was concentrated under reduced pressure, and thus obtained residue
  5. customwas purified by preparative thin-layer chromatography