Benzyl isocyanate → ethyl 2-(1-Methyl-2-(benzylcarbamoyl)hydrazinyl)acetate

HRID 576875ノート

反応式

HRID 576875 の反応式
[CH3:1][N:2]([CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])[NH2:3].[CH2:10]([N:17]=[C:18]=[O:19])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1>O1CCCC1.C(OCC)(=O)C>[CH3:1][N:2]([CH2:4][C:5]([O:7][CH2:8][CH3:9])=[O:6])[NH:3][C:18](=[O:19])[NH:17][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

参加物

5

反応物 2

HCID 76639Benzyl isocyanateHCID 20288078Ethyl 2-(1-methylhydrazinyl)acetate

生成物 1

HCID 66977957ethyl 2-(1-Methyl-2-(benzylcarbamoyl)hydrazinyl)acetate収率 76%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of ethyl 2-(1-methylhydrazinyl)acetate (Compound XL-1) 10 ml (76 mmol) in tetrahydrofuran 40 ml, benzyl isocyanate 11.1 g (83.3 mmol) was added at 0° C. and the mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate 150 ml and washed with water 75 ml and brine 75 ml. The organic phase was dried over magnesium sulfate and filtered. The filtrate was concentrated in vacuo to obtain the title compound 15.2 g (76%).

後処理

  1. washwashed with water 75 ml and brine 75 ml
  2. dry with materialThe organic phase was dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-e456841d45a84c60b5e7cea3ed743214
出典データセット
uspto-grants-2015_05
特許番号
US09040531B2

反応ノート

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