1,2-Dichloroethane → N'1,N'3-dimethyl-2-(2-methylhydrazono)-N'1,N'3-di(phenylcarbonoselenoyl)malonohydrazide

HRID 1401878ノート

反応式

HRID 1401878 の反応式
[CH3:1][N:2]([C:4](=[Se:11])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[NH2:3].[CH3:12][NH:13][N:14]=[C:15]([C:19]([OH:21])=O)[C:16](O)=[O:17].[CH2:22](Cl)[CH2:23]Cl>C(Cl)Cl>[CH3:1][N:2]([C:4]([C:23]1[CH:22]=[CH:7][CH:6]=[CH:5][CH:10]=1)=[Se:11])[NH:3][C:16](=[O:17])[C:15](=[N:14][NH:13][CH3:12])[C:19]([NH:3][N:2]([CH3:1])[C:4]([C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1)=[Se:11])=[O:21]

参加物

5

反応物 3

HCID 111,2-DichloroethaneHCID 553007652-(2-Methylhydrazono)malonic acidHCID 57551066N-methylbenzoselenohydrazide

生成物 1

HCID 25117166N'1,N'3-dimethyl-2-(2-methylhydrazono)-N'1,N'3-di(phenylcarbonoselenoyl)malonohydrazide収率 61.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of N-methylbenzoselenohydrazide, (430 mg, 2.0 mmol) and 2-(2-methylhydrazono)malonic acid (146 mg, 1.0 mmol) in CH2Cl2 (10 mL), was added EDC (480 mg, 2.5 mmol). The mixture was stirred for 1 h at RT. The reaction mixture was diluted with CH2Cl2 (25 mL) and washed with water and brine. The organic layer was dried over MgSO4 and filtered. After removal of the solvent, the product was purified by chromatography column on silica gel (1:1 Hexane:EtOAc and EtOAc) and to give N′1,N′3-dimethyl-2-(2-methylhydrazono)-N′1,N′3-di(phenylcarbonoselenoyl)malonohydrazide; (Compound 13) (330 mg) in 61.5% yield.

後処理

  1. washwashed with water and brine
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. customAfter removal of the solvent
  5. customthe product was purified by chromatography column on silica gel (1:1 Hexane:EtOAc and EtOAc)

出典と根拠

ORDレコード
ord-ea8f9881552b4f45828e357a543fba82
出典データセット
uspto-grants-2014_12
特許番号
US08907131B2

反応ノート

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