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Triethylamine → HCID 10194939, 화합물

HRID 1444000
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HRID 1444000 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].Cl.[NH:32]1[CH2:35][CH:34]([OH:36])[CH2:33]1.C(N([CH2:42][CH3:43])CC)C>C(#N)C.O>[C:34]([O:36][CH2:42][CH3:43])(=[O:10])[CH3:35].[CH3:4][CH2:5][CH2:6][CH:7]([CH3:2])[CH3:33].[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][CH:5]=[CH:4][C:3]=1[S:9]([NH:12][C:21]1[C:26]([O:27][CH3:28])=[N:25][C:24]([N:32]2[CH2:35][CH:34]([OH:36])[CH2:33]2)=[C:23]([Cl:30])[N:22]=1)(=[O:10])=[O:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 27592903-Hydroxyazetidine hydrochlorideHCID 11180148HCID 11180148, 화합물

생성물 2

HCID 10194939HCID 10194939, 화합물HCID 21882781Isohexane ethyl acetate

시약·촉매·용매 2

HCID 962Water용매
HCID 6342
Acetonitrile
용매

실험 절차

2,3-Dichloro-N-(5,6-dichloro-3-methoxy-2-pyrazinyl)-N-{[2-(trimethylsilyl)ethoxy]methyl}benzenesulphonamide (Example 66 part a) (0.20 g), azetidin-3-ol hydrochloride (0.082 g) and triethylamine (0.25 mL) in acetonitrile (3 mL) and water (0.5 mL) was stirred at room temperature. After 2 h, the mixture was evaporated and triturated with diethyl ether. The ethereal solution was evaporated and the residue dissolved in a 1 molar solution of tetrabutylammonium fluoride in THF (6 mL). After 16 h, the reaction mixture was concentrated and chromatography on silica gel eluting with ethyl acetate/isohexane mixtures gave the title compound as a white solid (0.024 g).

후처리

  1. customthe mixture was evaporated
  2. customtriturated with diethyl ether
  3. customThe ethereal solution was evaporated
  4. dissolutionthe residue dissolved in a 1 molar solution of tetrabutylammonium fluoride in THF (6 mL)
  5. waitAfter 16 h
  6. concentrationthe reaction mixture was concentrated

출처 및 근거

ORD 기록
ord-a9d8aec65a644f55a97abfb1b286dace
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07662825B2

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