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

HRID 1401878노트

반응식

HRID 1401878 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-ea8f9881552b4f45828e357a543fba82
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08907131B2

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