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4-Nitrobenzenesulfonyl chloride → HCID 694602, 화합물

HRID 1398070
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HRID 1398070 반응식
[N:1]1([CH2:7][CH2:8][OH:9])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[N+:10]([C:13]1[CH:18]=[CH:17][C:16]([S:19](Cl)(=[O:21])=[O:20])=[CH:15][CH:14]=1)([O-:12])=[O:11].C(N(CC)CC)C>ClCCl>[N+:10]([C:13]1[CH:14]=[CH:15][C:16]([S:19]([N:4]2[CH2:5][CH2:6][N:1]([CH2:7][CH2:8][OH:9])[CH2:2][CH2:3]2)(=[O:21])=[O:20])=[CH:17][CH:18]=1)([O-:12])=[O:11]
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참가 물질

5

반응물 3

HCID 74044-Nitrobenzenesulfonyl chlorideHCID 76771-(2-Hydroxyethyl)piperazineHCID 8471Triethylamine

생성물 1

HCID 694602HCID 694602, 화합물수율 94%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 415 μL (3.38 mmol) of 1-piperazineethanol in 20 mL of dichloromethane were added 500 mg (2.26 mmol) of 4-nitrobenzenesulfonyl chloride and 472 μL (3.38 mmol) of triethylamine under ice cooling, and the mixture was stirred for 30 minutes at the same temperature. The reaction mixture was diluted with dichloromethane and the organic layer was washed with water, saturated sodium bicarbonate aqueous solution and saturated saline solution and then, dried over with anhydrous sodium sulfate. The solvent was removed under reduced pressure and the residue was purified by silica gel column chromatography (eluent: dichloromethane/methanol=30/1) to give 670 mg (94%) of the title compound.

후처리

  1. washthe organic layer was washed with water, saturated sodium bicarbonate aqueous solution and saturated saline solution
  2. dry with materialdried over with anhydrous sodium sulfate
  3. customThe solvent was removed under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (eluent: dichloromethane/methanol=30/1)

출처 및 근거

ORD 기록
ord-ac3cd02972f54adc87658a0affb5461d
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08901315B2

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