Sodium hydride → Benzyl 4-amino-3-oxopiperazine-1-carboxylate

HRID 2086229ノート

反応式

HRID 2086229 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][NH:14][C:13](=[O:17])[CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H-].[Na+].C1(P(C2C=CC=CC=2)(O[NH2:29])=O)C=CC=CC=1>CN(C=O)C>[NH2:29][N:14]1[CH2:15][CH2:16][N:11]([C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[O:10])[CH2:12][C:13]1=[O:17]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 736777Benzyl 3-oxopiperazine-1-carboxylateHCID 10955453O-(Diphenylphosphinyl)hydroxylamine

生成物 1

HCID 22727156Benzyl 4-amino-3-oxopiperazine-1-carboxylate収率 96.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4-(Benzyloxycarbonyl)-2-piperazinone (4.685 g) was dissolved in DMF (170 ml) and combined with sodium hydride (800 mg, in oil) with cooling on ice. After stirring at room temperature for 30 minutes, O-diphenylphosphinyl hydroxylamine (4.896 g) was added and the mixture was stirred at 50° C. for 15 hours. The reaction mixture was concentrated under reduced pressure, and the residue was combined with aqueous sodium bicarbonate and extracted with dichloromethane. The extract was dried and concentrated to obtain the title compound 1-amino-4-benzyloxycarbonyl-2-piperazinone (4.8 g) as a colorless oil.

後処理

  1. temperaturewith cooling on ice
  2. stirringthe mixture was stirred at 50° C. for 15 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. extractionextracted with dichloromethane
  5. customThe extract was dried
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-328225b4edb24604a071d2160f817db0
出典データセット
uspto-grants-2004_04
特許番号
US06723722B1

反応ノート

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