tert-Butyl bromoacetate → 2-[5-[4-(t-Butoxycarbonylmethyl)hexahydro-1,4-diazepin-1-yl]pyrazin-2-ylcarbonylamino]-5-fluoro-N-(5-chloropyridin-2-yl)benzamide

HRID 1372879

反応式

HRID 1372879 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([NH:18][C:19]([C:21]2[CH:26]=[N:25][C:24]([N:27]3[CH2:33][CH2:32][CH2:31][NH:30][CH2:29][CH2:28]3)=[CH:23][N:22]=2)=[O:20])=[C:6]([CH:17]=1)[C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][N:11]=1)=[O:8].C(N(CC)C(C)C)(C)C.Br[CH2:44][C:45]([O:47][C:48]([CH3:51])([CH3:50])[CH3:49])=[O:46]>C(Cl)Cl.[Cl-].C[N+](CCCC)(CCCC)CCCC>[C:48]([O:47][C:45]([CH2:44][N:30]1[CH2:31][CH2:32][CH2:33][N:27]([C:24]2[N:25]=[CH:26][C:21]([C:19]([NH:18][C:5]3[CH:4]=[CH:3][C:2]([F:1])=[CH:17][C:6]=3[C:7]([NH:9][C:10]3[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][N:11]=3)=[O:8])=[O:20])=[N:22][CH:23]=2)[CH2:28][CH2:29]1)=[O:46])([CH3:51])([CH3:50])[CH3:49]

参加物

6

反応物 3

HCID 79177tert-Butyl bromoacetateHCID 81531DiisopropylethylamineHCID 98693075-Fluoro-2-[5-(hexahydro-1,4-diazepin-1-yl)pyrazin-2-yl-carbonylamino]-N-(5-chloropyridin-2-yl)benzamide

生成物 1

HCID 210727052-[5-[4-(t-Butoxycarbonylmethyl)hexahydro-1,4-diazepin-1-yl]pyrazin-2-ylcarbonylamino]-5-fluoro-N-(5-chloropyridin-2-yl)benzamide

試薬・触媒・溶媒 2

HCID 91822Tributylmethylammonium chloride触媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 5-fluoro-2-[5-(hexahydro-1,4-diazepin-1-yl)pyrazin-2-ylcarbonylamino]-N-(5-chloropyridin-2-yl)-benzamide (Example 1, 0.3 g, 0.64 mmol) in methylene chloride was added methyltributylammonium chloride (1 mL), N,N-diisopropylethylamine (2.2 mL) and tert-butyl bromoacetate (2.496 g). The mixture was stirred at room temperature until a clear solution was obtained (24–48 h), diluted with methylene chloride (50 mL), washed with water (2×10 mL) and brine, dried over sodium sulfate, evaporated, and dried. Yield=0.079 g.

後処理

  1. customwas obtained (24–48 h)
  2. washwashed with water (2×10 mL) and brine
  3. dry with materialdried over sodium sulfate
  4. customevaporated
  5. customdried

出典と根拠

ORDレコード
ord-7d74367f523a4ffe9b2b170a3420124e
出典データセット
uspto-grants-2007_01
特許番号
US07160878B2

関連ノート

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