反应 #463607

ord-88f5d475501241098154bbe215df8e61

反应方程式

CN(C)CCNS(=O)(=O)Cl
(2-dimethylaminoethyl)sulfamoyl chloride
CCCCCCCC/C=C\CCCCCCCCOCC(CO)OCCCCCCCC/C=C\CCCCCCCC
1,2-O-dioleylglycerol
CCCCCCCC/C=C\CCCCCCCCOCC(COS(=O)(=O)NCCN(C)C)OCCCCCCCC/C=C\CCCCCCCC
title compound
收率 18.3%
CCCCCCCC/C=C\CCCCCCCCOCC(COS(=O)(=O)NCCN(C)C)OCCCCCCCC/C=C\CCCCCCCC
3-O-(2-dimethylaminoethyl)sulfamoyl-1,2-O-dioleylglycerol
收率 18.3%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他After completion of the reaction
  2. 2
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure
  3. 3
    workup.ADDITIONthe residue was treated with methylene chloride-saturated aqueous sodium hydrogen carbonate solution
  4. 4
    干燥The methylene chloride layer was dried over sodium sulfate
  5. 5
    浓缩concentrated under reduced pressure

实验过程

In 4 ml of methylene chloride-pyridine (2:1) was dissolved 150 mg (0.25 mmol) of 1,2-O-dioleylglycerol. Then, 1 ml of a solution of 150 mg (0.75 mmol) (2-dimethylaminoethyl)sulfamoyl chloride in methylene chloride was added and the reaction was carried out at ambient temperature for 2 hours. After completion of the reaction, the solvent was distilled off under reduced pressure and the residue was treated with methylene chloride-saturated aqueous sodium hydrogen carbonate solution. The methylene chloride layer was dried over sodium sulfate and concentrated under reduced pressure. The residue was subjected to column chromatography (silica gel/methylene chloride-methanol) to provide 34 mg (18%) of the title compound of the invention.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06020317uspto-grants-2000_02