Sodium Hydroxide → 4-(4-Methoxybenzenesulfonyl)-1-(2-methyl-5-fluorobenzoyl)-2,3,4,5-tetrahydro-1H-[1,4]benzodiazepine-3-carboxylic Acid

HRID 1264589ノート

反応式

HRID 1264589 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([S:9]([N:12]2[CH2:18][C:17]3[CH:19]=[CH:20][CH:21]=[CH:22][C:16]=3[N:15]([C:23](=[O:32])[C:24]3[CH:29]=[C:28]([F:30])[CH:27]=[CH:26][C:25]=3[CH3:31])[CH2:14][CH:13]2[C:33]([O:35]C)=[O:34])(=[O:11])=[O:10])=[CH:5][CH:4]=1.[OH-].[Na+]>O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([S:9]([N:12]2[CH2:18][C:17]3[CH:19]=[CH:20][CH:21]=[CH:22][C:16]=3[N:15]([C:23](=[O:32])[C:24]3[CH:29]=[C:28]([F:30])[CH:27]=[CH:26][C:25]=3[CH3:31])[CH2:14][CH:13]2[C:33]([OH:35])=[O:34])(=[O:10])=[O:11])=[CH:7][CH:8]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 18612872Methyl 4-(4-Methoxybenzenesulfonyl)-1-(2-methyl-5-fluorobenzoyl)-2,3,4,5-tetrahydro-1H-[1,4]benzodiazepine-3-carboxylate

生成物 1

HCID 186129064-(4-Methoxybenzenesulfonyl)-1-(2-methyl-5-fluorobenzoyl)-2,3,4,5-tetrahydro-1H-[1,4]benzodiazepine-3-carboxylic Acid収率 76.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a mixture of 1.9 g (3.71 mmol) of methyl 4-(4-methoxybenzenesulfonyl)-1-(2-methyl-5-fluorobenzoyl)-2,3,4,5-tetrahydro-1H-[1,4]benzodiazepine-3-carboxylate in 10 ml of tetrahydrofuran was added 5 ml (4.82 mmol) of 1 N NaOH. The mixture was stirred at room temperature for 1.5 hours and the solvent removed under vacuum. To the residue was added ethyl acetate and the mixture neutralized with 1 N HCl. The organic layer was separated, washed with brine and dried with Na2SO4. The solvent was removed under vacuum to give 1.41 g of white solid. Anal. for C25H23FN2O6S: Calc'd: C, 60.2; H, 4.7; N, 5.6; Found: C, 60.2; H, 4.8; N, 5.4 S, 6.4; F, 3.6.

後処理

  1. customthe solvent removed under vacuum
  2. additionTo the residue was added ethyl acetate
  3. customThe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried with Na2SO4
  6. customThe solvent was removed under vacuum

出典と根拠

ORDレコード
ord-54d22cdbb0814144ba5964369190c587
出典データセット
uspto-grants-2003_04
特許番号
US06544984B1

反応ノート

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