Acetic Anhydride → HCID 86758535、化合物

HRID 989638ノート

反応式

HRID 989638 の反応式
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[NH:13][CH:12]([CH2:14][C:15]([O:17][CH3:18])=[O:16])[C:11](=[O:19])[N:10]([CH3:20])[CH2:9][C:8]=2[CH:21]=1)([OH:3])=[O:2].[C:22](OC(=O)C)(=[O:24])[CH3:23]>C(O)(=O)C>[C:22]([N:13]1[C:7]2[CH:6]=[CH:5][C:4]([C:1]([OH:3])=[O:2])=[CH:21][C:8]=2[CH2:9][N:10]([CH3:20])[C:11](=[O:19])[CH:12]1[CH2:14][C:15]([O:17][CH3:18])=[O:16])(=[O:24])[CH3:23]

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 23505570Methyl 7-carboxy-2,3,4,5-tetrahydro-4-methyl-3-oxo-1h-1,4-benzodiazepine-2-acetate

生成物 1

HCID 86758535HCID 86758535、化合物収率 78%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Methyl (±)-7-carboxy-4-methyl-3-oxo-2,3,4,5-tetrahydro-1H-1,4-benzodiazepine-2-acetate (2.0 g, 8.6 mmol), acetic anhydride (25 mL) and acetic acid (1 mL) were heated to reflux. After 48 h, the reaction was concentrated, and the residue was diluted with H2O (20 mL) and MeOH (15 mL). The resulting solution was concentrated to give the tide compound (1.8 g, 78%): 1H NMR (400 MHz, DMSO-d6) δ1.7-1.8 (s, 3H), 2.2-2.6 (m, 2H), 2.9-3.0 (s, 3H), 3.5-3.6 (s, 3H), 4.2-4.3 (d, 1H), 4.7-4.8 (d, 1H), 5.8-5.9 (t, 1H), 7.5-7.6 (d, 1H), 7.9-8.0 (dd, 1H), 8.1-8.2 (d, 1H); MS (ES) m/e 335.0 (M+H)+.

後処理

  1. concentrationthe reaction was concentrated
  2. additionthe residue was diluted with H2O (20 mL) and MeOH (15 mL)
  3. concentrationThe resulting solution was concentrated

出典と根拠

ORDレコード
ord-421df1a9e3df4e5f86ec15020b8a258b
出典データセット
uspto-grants-2002_10
特許番号
US06458784B1

反応ノート

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