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Diisopropylethylamine → HCID 178442204, 화합물

HRID 2113504
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HRID 2113504 반응식
[N:1]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[C:7]1[NH:11][N:10]=[C:9]([C:12]2[S:13][CH:14]=[CH:15][CH:16]=2)[C:8]=1[CH2:17][CH2:18][NH2:19].C(N(C(C)C)CC)(C)C.[CH2:29]([C:34]1[CH:39]=[CH:38][C:37]([S:40](Cl)(=[O:42])=[O:41])=[CH:36][CH:35]=1)[CH2:30][CH2:31][CH2:32][CH3:33]>ClCCl>[CH2:29]([C:34]1[CH:35]=[CH:36][C:37]([S:40]([NH:19][CH2:18][CH2:17][C:8]2[C:9]([C:12]3[S:13][CH:14]=[CH:15][CH:16]=3)=[N:10][NH:11][C:7]=2[C:2]2[CH:3]=[N:4][CH:5]=[CH:6][N:1]=2)(=[O:42])=[O:41])=[CH:38][CH:39]=1)[CH2:30][CH2:31][CH2:32][CH3:33]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 1446254-t-Amylbenzenesulphonyl chlorideHCID 178510737HCID 178510737, 화합물

생성물 1

HCID 178442204HCID 178442204, 화합물수율 30,580.699%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of the 2-(5-Pyrazin-2-yl-3-thiophen-2-yl-1H-pyrazol-4-yl)-ethylamine 1D (7 mg, 25.8 μmol), diisopropylethylamine (9.0 μl, 51.6 μmol) and 4-n-pentylbenzenesulfonyl chloride (7.0 mg, 28.3 μmol) in dichloromethane (1 mL) was stirred for 3 h. The reaction mixture was concentrated under reduced pressure. The crude product dissolved in methanol (2 ml) and was purified by prep-HPLC. Removal of the solvent in vacuo provided the title compound (3.8 g mg, 41% yield). MS m/e 481; HPLC retention time 3.54 min (Method A).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionThe crude product dissolved in methanol (2 ml)
  3. customwas purified by prep-HPLC
  4. customRemoval of the solvent in vacuo

출처 및 근거

ORD 기록
ord-9245dadad15f431a98c92fe503e58551
출처 데이터셋
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07432271B2

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