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HCID 18378637、化合物 → HCID 86758696、化合物

HRID 2298803
ノート
印刷プレビュー

反応式

HRID 2298803 の反応式
[CH3:1][O:2][CH:3]1[C:11](=[C:12]=[O:13])[C:10]([N:14]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[CH2:18][CH2:17][CH2:16][CH2:15]2)=[CH:9][CH:8]=[C:4]1[C:5]([OH:7])=O.[NH2:25][C:26]1[C:34]2[N:33]=[C:32]([CH3:35])[N:31]([C:36]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37])[C:30]=2[CH:29]=[CH:28][CH:27]=1.OS1C2C=CC=CC=2N=C1>CN(C)C=O.C(OCC)(=O)C>[CH3:1][O:2][CH:3]1[C:11](=[C:12]=[O:13])[C:10]([N:14]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[CH2:18][CH2:17][CH2:16][CH2:15]2)=[CH:9][CH:8]=[C:4]1[C:5]([NH:25][C:26]1[C:34]2[N:33]=[C:32]([CH3:35])[N:31]([C:36]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37])[C:30]=2[CH:29]=[CH:28][CH:27]=1)=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 18378637HCID 18378637、化合物HCID 86758697HCID 86758697、化合物HCID 178527226HCID 178527226、化合物

生成物 1

HCID 86758696HCID 86758696、化合物収率 54.3%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate
溶媒

実験手順

A mixture of 2-methoxy-4-(2,3,4,5-tetrahydro-1H-1-benzazepin-1-yl)-carbonylbenzoic acid (200 mg), 4-amino-1-tert-butoxycarbonyl-2-methyl-1H-benzimidazole (152 mg), WSCD·HCl [water soluble carbodiimide, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride, 141 mg] and 1-hydroxybenzotiazole (100 mg) in N,N-dimethylformamide (5 ml) was stirred at room temperature overnight, and the mixture was diluted with ethyl acetate. The solution was washed successively with saturated aqueous sodium hydrogencarbonate solution, water, and brine and dried over magnesium sulfate. The solvent was evaporated and the residue was purified by silica gel column chromatography using chloroform as an eluent to give 2-methoxy-N-[2-methyl-1-(tert-butoxycarbonyl)-1H-benzimidazol-4-yl]-4-(2,3,4,5-tetrahydro-1H-1-benzazepin-1-yl)-carbonylbenzamide (185 mg).

後処理

  1. washThe solution was washed successively with saturated aqueous sodium hydrogencarbonate solution, water, and brine
  2. dry with materialdried over magnesium sulfate
  3. customThe solvent was evaporated
  4. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-9a7a0bb4eff347b29defd26a4f3e34bd
出典データセット
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06495542B1

反応ノート

読み込み中…

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