Sodium Hydroxide → 1-methoxycarbonyl-7-(4-morpholinophenyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid

HRID 586866ノート

反応式

HRID 586866 の反応式
[CH3:1][O:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][C:14]([C:16]3[CH:21]=[CH:20][C:19]([N:22]4[CH2:27][CH2:26][O:25][CH2:24][CH2:23]4)=[CH:18][CH:17]=3)=[CH:15][C:10]=2[CH:9]=[C:8]([C:28]([O:30]C)=[O:29])[CH2:7][CH2:6]1)=[O:4].[OH-].[Na+]>CO.C1COCC1>[CH3:1][O:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][C:14]([C:16]3[CH:17]=[CH:18][C:19]([N:22]4[CH2:27][CH2:26][O:25][CH2:24][CH2:23]4)=[CH:20][CH:21]=3)=[CH:15][C:10]=2[CH:9]=[C:8]([C:28]([OH:30])=[O:29])[CH2:7][CH2:6]1)=[O:4]

参加物

5

反応物 2

HCID 14798Sodium Hydroxide2 回HCID 22328989HCID 22328989、化合物

生成物 1

HCID 223292091-methoxycarbonyl-7-(4-morpholinophenyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid収率 96.8%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

In methanol (40 ml) and THF (60 ml) was dissolved methyl 1-methoxycarbonyl-7-(4-morpholinophenyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylate (0.31 g). To the solution was-added 1N sodium hydroxide solution (5 ml), and the mixture was stirred at room temperature overnight. To the mixture was added 1N sodium hydroxide solution (2.5 ml), and the mixture was stirred at room temperature overnight and concentrated. The residue was neutralized with 1N hydrochloric acid, precipitated crystals were filtered and washed with water to give 1-methoxycarbonyl-7-(4-morpholinophenyl)-2,3-dihydro-1H-1-benzazepine-4-carboxylic acid (0.29 g) as colorless crystals.

後処理

  1. stirringthe mixture was stirred at room temperature overnight
  2. concentrationconcentrated
  3. customprecipitated crystals
  4. filtrationwere filtered
  5. washwashed with water

出典と根拠

ORDレコード
ord-c47cf545b6d744548bb8ecb121bde0dd
出典データセット
uspto-grants-2005_08
特許番号
US06936602B1

反応ノート

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