HRID227258

反应详情

EQUATION

反应方程式

HRID 227258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Triethylamine (0.12 ml, 0.89 mmol) and subsequently 4-chlorobenzenesulfonyl chloride (314 mg, 1.49 mmol) were added to a solution of 1,3-dibenzyl-1,4,8-triaza-spiro[4,5]decan-2-one (249 mg, 0.75 mmol) in CH2Cl2 (6.7 ml) with stirring under a blanket of nitrogen at RT. The reaction mixture was stirred overnight. The organic phase was rendered alkaline using saturated aqueous sodium carbonate solution (20 ml) and the aqueous phase was extracted with CH2Cl2 (15 ml). The combined organic phases were dried over Na2SO4. After filtration, removal of the solvent and column chromatography, the desired product 1,3-dibenzyl-8-(4-chlorobenzene-sulfonyl)-1,4,8-triazaspiro[4,5]decan-2-one was obtained in a yield of 382 mg (100% of theory).

WORKUP

后处理

  1. stirringThe reaction mixture was stirred overnight
  2. extractionthe aqueous phase was extracted with CH2Cl2 (15 ml)
  3. dry with materialThe combined organic phases were dried over Na2SO4
  4. filtrationAfter filtration, removal of the solvent and column chromatography