Hydrochloric Acid → 3-Benzyloxy-4-oxo-5,6,7,8-tetrahydro-4H-pyrazolo[1,5-a][1,4]diazepine-2-carboxylic acid

HRID 1453867ノート

反応式

HRID 1453867 の反応式
[CH2:1]([O:8][C:9]1[C:10]([C:20]([O:22]C)=[O:21])=[N:11][N:12]2[CH2:18][CH2:17][CH2:16][NH:15][C:14](=[O:19])[C:13]=12)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].Cl>CO>[CH2:1]([O:8][C:9]1[C:10]([C:20]([OH:22])=[O:21])=[N:11][N:12]2[CH2:18][CH2:17][CH2:16][NH:15][C:14](=[O:19])[C:13]=12)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2 回HCID 68952653Methyl 3-benzyloxy-4-oxo-5,6,7,8-tetrahydro-4H-pyrazolo[1,5-a][1,4]diazepine-2-carboxylate

生成物 1

HCID 689526853-Benzyloxy-4-oxo-5,6,7,8-tetrahydro-4H-pyrazolo[1,5-a][1,4]diazepine-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of methyl 3-benzyloxy-4-oxo-5,6,7,8-tetrahydro-4H-pyrazolo[1,5-a][1,4]diazepine-2-carboxylate (50 mg, 0.159 mmol) in MeOH (2 mL) was added aqueous 1M NaOH (159 μL, 0.159 mmol). The reaction was stirred at room temperature for 4 hours, treated with additional aqueous 1N NaOH (159 μL, 0.159 mmol), and stirred at room temperature overnight. Aqueous 1N HCl (318 μL, 0.318 mmol) was added to the solution, and the solvents were removed in vacuo to afford the title product. 1H NMR (400 MHz, CD3OD) δ 7.39-7.36 (m, 2H), 7.32-7.28 (m, 3H), 5.24 (s, 3H), 4.38-4.34 (t, 2H), 2.90-2.86 (t, 2H), 2.13-2.06 (dt, 2H); ES MS (M+1)=302.

後処理

  1. stirringstirred at room temperature overnight
  2. customthe solvents were removed in vacuo

出典と根拠

ORDレコード
ord-cb260ec7960746afadfbe1059bc3d7d3
出典データセット
uspto-grants-2009_01
特許番号
US07476666B2

反応ノート

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