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1,2-Dichloroethane → 4-[4-(1-Oxo-but-2-ynylamino)-benzenesulfonyl]-piperazine-1-carboxylic acid tert-butyl ester

HRID 1841918
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HRID 1841918 반응식
[C:1]([OH:6])(=O)[C:2]#[C:3][CH3:4].N1C=CC=CC=1.[C:13]([O:17][C:18]([N:20]1[CH2:25][CH2:24][N:23]([S:26]([C:29]2[CH:34]=[CH:33][C:32]([NH2:35])=[CH:31][CH:30]=2)(=[O:28])=[O:27])[CH2:22][CH2:21]1)=[O:19])([CH3:16])([CH3:15])[CH3:14].C(Cl)CCl>C1COCC1.CC(N(C)C)=O.C(OCC)(=O)C>[C:13]([O:17][C:18]([N:20]1[CH2:25][CH2:24][N:23]([S:26]([C:29]2[CH:30]=[CH:31][C:32]([NH:35][C:1](=[O:6])[C:2]#[C:3][CH3:4])=[CH:33][CH:34]=2)(=[O:28])=[O:27])[CH2:22][CH2:21]1)=[O:19])([CH3:16])([CH3:14])[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 111,2-DichloroethaneHCID 1049PyridineHCID 685352-Butynoic acidHCID 10617209tert-Butyl 4-(4-aminophenylsulfonyl)piperazine-1-carboxylate

생성물 1

HCID 569547204-[4-(1-Oxo-but-2-ynylamino)-benzenesulfonyl]-piperazine-1-carboxylic acid tert-butyl ester수율 20.8%

시약·촉매·용매 2

HCID 8857
Ethyl Acetate
용매
HCID 69293768tetrahydrofuran N,N-dimethylacetamide용매

실험 절차

But-2-ynoic acid (0.19 g, 2.36 mmol) followed by pyridine (0.6 ml), were added sequentially portion wise to a stirred solution of 4-(4-amino-benzenesulfonyl)-piperazine-1-carboxylic acid tert-butyl ester (0.2 g, 0.59 mmol) in THF/DMA (3:2, 5 ml) at room temperature. To this mixture was added EDC (0.6 g, 3.1 mmol) in one portion and the mixture was stirred at room temperature under a nitrogen atmosphere for 1 hour. After this time the mixture was diluted with ethyl acetate (50 ml) and washed with water (100 ml), saturated NaHCO3 (100 ml) and HCl (100 ml, 2M). The organic layer was separated, dried (MgSO4), filtered and concentrated under vacuum and the resulting residue was purified by flash column chromatography (elution, 20% ethyl acetate, 80% DCM) to give the title compound (0.05 g, 19% yield) as a white solid. Tr=4.12 min, m/z (ES+) (M+Na)+ 430.

후처리

  1. washwashed with water (100 ml), saturated NaHCO3 (100 ml) and HCl (100 ml, 2M)
  2. customThe organic layer was separated
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum
  6. customthe resulting residue was purified by flash column chromatography (elution, 20% ethyl acetate, 80% DCM)

출처 및 근거

ORD 기록
ord-c8e797c64b3f47c9883cc0d88d728f0a
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946197B2

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