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2,4-Dimethoxybenzylamine → C-(3-Bromophenyl)-N-(2,4-dimethoxybenzyl)methanesulfonamide

HRID 339834
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HRID 339834 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:10]=[CH:11][CH:12]=1)[CH2:5][S:6](Cl)(=[O:8])=[O:7].[CH3:13][O:14][C:15]1[CH:22]=[C:21]([O:23][CH3:24])[CH:20]=[CH:19][C:16]=1[CH2:17][NH2:18]>ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([CH2:5][S:6]([NH:18][CH2:17][C:16]2[CH:19]=[CH:20][C:21]([O:23][CH3:24])=[CH:22][C:15]=2[O:14][CH3:13])(=[O:8])=[O:7])[CH:10]=[CH:11][CH:12]=1
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참가 물질

4

반응물 2

HCID 5972502,4-DimethoxybenzylamineHCID 2761451(3-bromophenyl)methanesulfonyl Chloride

생성물 1

HCID 68292274C-(3-Bromophenyl)-N-(2,4-dimethoxybenzyl)methanesulfonamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

While cooling with ice, 9.90 g of 3-bromobenzylsulfonyl chloride were initially charged in 120 ml of dichloromethane, and a solution of 11.55 ml of 2,4-dimethoxybenzylamine in 60 ml of dichloromethane was added dropwise within 15 minutes. The reaction mixture was allowed to come to room temperature and stirred for 1 hour. Subsequently, the mixture was washed with 50 ml of water, with 100 ml of 1 N aqueous hydrochloric acid, with 100 ml of saturated aqueous sodium hydrogencarbonate solution and finally once more with 100 ml of water. The organic phase was dried over MgSO4 and concentrated by rotary evaporation. The residue (14.30 g) was used in the next reaction without further purification.

후처리

  1. customto come to room temperature
  2. washSubsequently, the mixture was washed with 50 ml of water, with 100 ml of 1 N aqueous hydrochloric acid, with 100 ml of saturated aqueous sodium hydrogencarbonate solution and finally once more with 100 ml of water
  3. dry with materialThe organic phase was dried over MgSO4
  4. concentrationconcentrated by rotary evaporation
  5. customThe residue (14.30 g) was used in the next reaction without further purification

출처 및 근거

ORD 기록
ord-ea1f3e3aa0b049579333607fb37f4ba8
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08895547B2

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