2-Aminothiazole → HCID 86653790、化合物

HRID 85117

反応式

HRID 85117 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:12][CH2:11][CH:10]([O:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=2[C:20]2[NH:24][C:23]3[CH:25]=[CH:26][CH:27]=[C:28]([C:29](O)=[O:30])[C:22]=3[N:21]=2)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[S:32]1[CH:36]=[CH:35][N:34]=[C:33]1[NH2:37].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C.O>[S:32]1[CH:36]=[CH:35][N:34]=[C:33]1[NH:37][C:29]([C:28]1[C:22]2[N:21]=[C:20]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[O:13][CH:10]3[CH2:11][CH2:12][N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[CH2:9]3)[NH:24][C:23]=2[CH:25]=[CH:26][CH:27]=1)=[O:30]

参加物

7

反応物 4

HCID 21552-AminothiazoleHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 672015052-(2-(1-(tert-butoxycarbonyl)pyrrolidin-3-yloxy)phenyl)-1H-benzo[d]imidazole-4-carboxylic acid

生成物 1

HCID 86653790HCID 86653790、化合物収率 48%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 2-(2-(1-(tert-butoxycarbonyl)pyrrolidin-3-yloxy)phenyl)-1H-benzo[d]imidazole-4-carboxylic acid (31; 150 mg, 0.36 mmol), thiazol-2-amine (4; 35.5 mg, 0.36 mmol), and HATU (202 mg, 0.53 mmol) in DMF (5 mL) was added DIEA (137 mg, 1.06 mmol). The mixture was stirred at room temperature for 18 h. It was then diluted with water (20 mL) and stirred for 30 min. The precipitate was collected by filtration, and then purified by column chromatography to give 85 mg of the title compound 32 (yield: 48%). MS (ESI) calcd for C26H27N5O4S: 505.18; found: 506 [M+H].

後処理

  1. stirringstirred for 30 min
  2. filtrationThe precipitate was collected by filtration
  3. custompurified by column chromatography

出典と根拠

ORDレコード
ord-989dc590c2ba425ea577f04c9b5db245
出典データセット
uspto-grants-2014_09
特許番号
US08846947B2

関連ノート

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