Dimethylamine → N,N-dimethyl-4-nitrobenzenesulfonamide

HRID 1484831

반응식

HRID 1484831 반응식
[CH3:1][NH:2][CH3:3].CCN(C(C)C)C(C)C.[N+:13]([C:16]1[CH:21]=[CH:20][C:19]([S:22](Cl)(=[O:24])=[O:23])=[CH:18][CH:17]=1)([O-:15])=[O:14]>C(Cl)Cl>[CH3:1][N:2]([CH3:3])[S:22]([C:19]1[CH:18]=[CH:17][C:16]([N+:13]([O-:15])=[O:14])=[CH:21][CH:20]=1)(=[O:23])=[O:24]

참가 물질

5

반응물 3

HCID 674DimethylamineHCID 74044-Nitrobenzenesulfonyl chlorideHCID 81531Diisopropylethylamine

생성물 1

HCID 2747580N,N-dimethyl-4-nitrobenzenesulfonamide수율 91%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To the solution of dimethylamine (284 mg, 6.3 mmol, 1.5 equiv.) and DIPEA (1 mL) in DCM (15 mL) was added dropwise a solution of 4-nitrobenzene-1-sulfonyl chloride (800 mg, 4.2 mmol, 1.0 equiv.) in DCM (5 mL). The reaction mixture was stirred at room temperature for 2 h. Then, the reaction mixture was washed with water and brine. The organic layers was dried (Na2SO4) and concentrated to get the residue, which was washed with isopropyl ether to afford compound N,N-dimethyl-4-nitrobenzenesulfonamide (879 mg, 91%).

후처리

  1. washThen, the reaction mixture was washed with water and brine
  2. dry with materialThe organic layers was dried (Na2SO4)
  3. concentrationconcentrated
  4. customto get the residue, which
  5. washwas washed with isopropyl ether

출처 및 근거

ORD 기록
ord-bb57abf62e43442b94674328fd6e7599
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09422271B2

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