Triethylamine → Benzenesulfonamide

HRID 481986

반응식

HRID 481986 반응식
CS(Cl)(=O)=O.OCC[N:9](CCO)[S:10]([C:13]1[CH:18]=[CH:17][C:16](C)=[CH:15][CH:14]=1)(=[O:12])=[O:11].C(N(CC)CC)C>ClCCl>[C:13]1([S:10]([NH2:9])(=[O:12])=[O:11])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 81565N,N-Bis(2-hydroxyethyl)-4-methylbenzenesulfonamide

생성물 1

HCID 7370Benzenesulfonamide수율 85.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 11.4 g (0.1 mole) of methanesulfonyl chloride in 17.1 ml of dichloromethane is cooled to 5° C. A solution of 13 g (0.05 mole) of N,N-bis(2-hydroxyethyl)-4-methylbenzenesulfonamide and 10.1 g (0.1 mole) of triethylamine in 52 ml of dichloromethane is then added dropwise with stirring. The resulting mixture is allowed to return to ambient temperature and stirred for a further 3 hours. The reaction mixture is then extracted three times with 40 ml water. The organic phase is dried over sodium sulfate, filtered and concentrated in a rotating evaporator. The resulting oil is then crystallized from ethanol. 17.8 g of 4-methyl-N,N-bis[2-methylsulfonyloxy)ethyl]benzenesulfonamide are obtained.

후처리

  1. customto return to ambient temperature
  2. stirringstirred for a further 3 hours
  3. extractionThe reaction mixture is then extracted three times with 40 ml water
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in a rotating evaporator
  7. customThe resulting oil is then crystallized from ethanol

출처 및 근거

ORD 기록
ord-ccc72a90f7184e26b8ea2436581a081a
출처 데이터셋
uspto-grants-1998_08
특허 번호
US05792770

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