4-Toluenesulfonyl chloride → N,N-bis(2-(p-toluenesulfonyloxy)ethyl)-p-toluenesulfonamide

HRID 728631

반응식

HRID 728631 반응식
[NH:1]([CH2:5][CH2:6][OH:7])[CH2:2][CH2:3][OH:4].[S:8](Cl)([C:11]1[CH:17]=[CH:16][C:14]([CH3:15])=[CH:13][CH:12]=1)(=[O:10])=[O:9]>N1C=CC=CC=1>[S:8]([N:1]([CH2:5][CH2:6][O:7][S:8]([C:11]1[CH:17]=[CH:16][C:14]([CH3:15])=[CH:13][CH:12]=1)(=[O:10])=[O:9])[CH2:2][CH2:3][O:4][S:8]([C:11]1[CH:17]=[CH:16][C:14]([CH3:15])=[CH:13][CH:12]=1)(=[O:10])=[O:9])([C:11]1[CH:17]=[CH:16][C:14]([CH3:15])=[CH:13][CH:12]=1)(=[O:10])=[O:9]

참가 물질

4

반응물 2

HCID 73974-Toluenesulfonyl chlorideHCID 8113Diethanolamine

생성물 1

HCID 267409N,N-bis(2-(p-toluenesulfonyloxy)ethyl)-p-toluenesulfonamide수율 85%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

A solution of 32.5 g (0.31 mole) of diethanolamine in 60 cm3 of pyridine are added slowly to a solution of 185 g (0.97 mole) of tosyl chloride in 220 cm3 of pyridine at 0° C. so that the temperature does not exceed 5° C. After the addition is complete, the mixture is maintained at this temperature for 1 h, then it is poured into 220 cm3 of ice-cold water with vigorous stirring. After filtration, washing and drying 148.4 g of precipitate are obtained (yield 85%; Rf=0.6 silica/CH2Cl2 /acetone/98/2).

후처리

  1. customdoes not exceed 5° C
  2. additionAfter the addition
  3. temperaturethe mixture is maintained at this temperature for 1 h
  4. filtrationAfter filtration
  5. washwashing
  6. dry with materialdrying 148.4 g of precipitate
  7. customare obtained (yield 85%; Rf=0.6 silica/CH2Cl2 /acetone/98/2)

출처 및 근거

ORD 기록
ord-5beef8f61e2749169ab4d1b52e210bd8
출처 데이터셋
uspto-grants-1991_09
특허 번호
US05049667

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