Benzenecarboximidic acid, 3-methoxy-, ethyl ester, hydrochloride → HCID 59519026、化合物

HRID 1161855ノート

反応式

HRID 1161855 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[CH:20]=[CH:19][C:18]([NH2:21])=[C:17]([C:22](=[O:31])[NH:23][CH2:24][C:25](=[O:30])[NH:26][CH:27]([CH3:29])[CH3:28])[CH:16]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.[CH3:33][O:34][C:35]1[CH:36]=[C:37]([CH:43]=[CH:44][CH:45]=1)[C:38](=N)OCC>CCO>[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][CH2:12][N:11]([C:15]2[CH:16]=[C:17]3[C:18](=[CH:19][CH:20]=2)[N:21]=[C:38]([C:37]2[CH:43]=[CH:44][CH:45]=[C:35]([O:34][CH3:33])[CH:36]=2)[N:23]([CH2:24][C:25](=[O:30])[NH:26][CH:27]([CH3:28])[CH3:29])[C:22]3=[O:31])[CH2:10][CH2:9]1)=[O:7])([CH3:2])([CH3:4])[CH3:3]

参加物

4

反応物 2

HCID 12282163Benzenecarboximidic acid, 3-methoxy-, ethyl ester, hydrochlorideHCID 67417372HCID 67417372、化合物

生成物 1

HCID 59519026HCID 59519026、化合物収率 13%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 4-{4-Amino-3-[(isopropylcarbamoylmethyl)carbamoyl]phenyl}perhydro-1,4-diazepine-1-carboxylic acid tert-butyl ester (INTERMEDIATE V.2) (300 mg, 0.69 mmol) and ethyl 3-methoxybenzimidate hydrochloride (INTERMEDIATE II.2) (298 mg, 1.38 mmol) in EtOH (6 mL) was heated at reflux temperature for 16 h. The reaction mixture was cooled, filtered and the filtrate concentrated in vacuo. The crude residue was purified by preparative HPLC to afford 4-[3-(isopropylcarbamoylmethyl)-2-(3-methoxyphenyl)-4-oxo-3,4-dihydroquinazolin-6-yl]perhydro-1,4-diazepine-1-carboxylic acid tert-butyl ester (INTERMEDIATE VII.1) (50 mg, 0.09 mmol, 13%).

後処理

  1. temperaturewas heated
  2. temperatureat reflux temperature for 16 h
  3. temperatureThe reaction mixture was cooled
  4. filtrationfiltered
  5. concentrationthe filtrate concentrated in vacuo
  6. customThe crude residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-09aeeba715524762bbccf20a604bc74f
出典データセット
uspto-grants-2010_10
特許番号
US07820649B2

反応ノート

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