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Triethylamine → HCID 59168104, 화합물

HRID 1443993
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HRID 1443993 반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[S:9]([N:12]([C:21]1[C:26]([O:27][CH3:28])=[N:25][C:24](Cl)=[C:23]([Cl:30])[N:22]=1)COCC[Si](C)(C)C)(=[O:11])=[O:10].[C:31]([NH:34][CH2:35][CH2:36][NH2:37])(=[O:33])[CH3:32].C(N(CC)CC)C>C(#N)C>[Cl:30][C:23]1[C:24]([NH:37][CH2:36][CH2:35][NH:34][C:31](=[O:33])[CH3:32])=[N:25][C:26]([O:27][CH3:28])=[C:21]([NH:12][S:9]([C:3]2[CH:4]=[CH:5][CH:6]=[C:7]([Cl:8])[C:2]=2[Cl:1])(=[O:10])=[O:11])[N:22]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 66082N-(2-aminoethyl)acetamideHCID 11180148HCID 11180148, 화합물

생성물 1

HCID 59168104HCID 59168104, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

2,3-Dichloro-N-(5,6-dichloro-3-methoxy-2-pyrazinyl)-N-{[2-(trimethylsilyl)ethoxy]methyl}benzenesulphonamide (Example 66 part a) (0.26 g) was dissolved in acetonitrile (1.0 mL) and N-acetylethylenediamine (0.055 mL) and triethylamine (0.19 mL) added. After 48 h, the reaction mixture was concentrated and chromatography on silica gel eluting with ethyl acetate gave the title compound protected with the SEM group, as an oil (0.13 g). The oil was dissolved in dichloromethane (2.0 mL) and boron trifluoride etherate (0.14ml) added. After 2 h, ethyl acetate (20 mL) was added and the mixture washed with 5% aqueous citric acid (5 mL), dried (MgSO4) and evaporated. Chromatography on silica gel eluting with ethyl acetate gave the title compound as a solid (0.031 g).

후처리

  1. concentrationthe reaction mixture was concentrated

출처 및 근거

ORD 기록
ord-4b31a4d70eaf4ceb8e077bc7b4d4c50a
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07662825B2

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