Triethylamine → HCID 58500436, 화합물

HRID 1907144노트

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HRID 1907144 반응식
[CH:1]([NH:4][C:5]([C:7]1[C:15]2[C:11](=[CH:12][NH:13][N:14]=2)[CH:10]=[C:9]([CH3:16])[C:8]=1[NH:17][C:18]([C:20]1[N:21]([C:27]2[C:32]([Cl:33])=[CH:31][CH:30]=[CH:29][N:28]=2)[N:22]=[C:23]([O:25][CH3:26])[CH:24]=1)=[O:19])=[O:6])([CH3:3])[CH3:2].[CH2:34]([O:36][C:37](=[O:43])[CH2:38][S:39][C:40](Cl)=[O:41])[CH3:35].C(N(CC)CC)C>C(Cl)(Cl)Cl>[CH2:34]([O:36][C:37](=[O:43])[CH2:38][S:39][C:40]([N:13]1[CH:12]=[C:11]2[C:15]([C:7]([C:5](=[O:6])[NH:4][CH:1]([CH3:3])[CH3:2])=[C:8]([NH:17][C:18]([C:20]3[N:21]([C:27]4[C:32]([Cl:33])=[CH:31][CH:30]=[CH:29][N:28]=4)[N:22]=[C:23]([O:25][CH3:26])[CH:24]=3)=[O:19])[C:9]([CH3:16])=[CH:10]2)=[N:14]1)=[O:41])[CH3:35]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 18958640Ethyl [(chlorocarbonyl)sulfanyl]acetateHCID 178492656HCID 178492656, 화합물

생성물 1

HCID 58500436HCID 58500436, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매2회

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온도
20 °C

실험 절차

In a vial, 6-{[2-(3-chloro-pyridin-2-yl)-5-methoxy-2H-pyrazole-3-carbonyl]-amino}-5-methyl-2H-indazole-7-carboxylic acid isopropyl amide (0.200 g, 0.427 mmol) was suspended in chloroform (1 ml), then a solution of (chlorocarbonylthio)-acetic acid ethyl ester (0.086 g, 0.471 mmol) in chloroform (1 ml) was added, followed by triethylamine (0.065 ml). The reaction mixture became a clear solution that was stirred for 1 hour at a temperature of 20° C. The reaction mixture was concentrated and the residue was purified by flash chromatography over silica gel using a 50% ethyl acetate-50% cyclohexane mixture. The desired compound was isolated as a yellow solid showing the physical properties reported in the corresponding table (P.41.).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. customthe residue was purified by flash chromatography over silica gel using a 50% ethyl acetate-50% cyclohexane mixture

출처 및 근거

ORD 기록
ord-239f40e833e143dea6f352564b5f3d2e
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08598078B2

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