Formamide → N-cyano-N'-[2-(3-formylamino-2-oxobutylthio)ethyl]-N"-methylguanidine

HRID 477283노트

반응식

HRID 477283 반응식
Cl[CH:2]([C:14](=O)[CH3:15])[CH2:3][S:4][CH2:5][CH2:6][NH:7][C:8]([NH:11][C:12]#[N:13])=[N:9][CH3:10].C([O-])=[O:18].[NH4+].C([O-])([O-])OC.O.O.O.O.P([O-])([O-])(O)=O.[NH4+].[Na+].[CH:37]([NH2:39])=[O:38].C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[C:12]([NH:11][C:8]([NH:7][CH2:6][CH2:5][S:4][CH2:3][C:2](=[O:18])[CH:14]([NH:39][CH:37]=[O:38])[CH3:15])=[N:9][CH3:10])#[N:13]

참가 물질

8

반응물 6

HCID 713FormamideHCID 516892Sodium BicarbonateHCID 2723923Ammonium formateHCID 14153741N-[2-(2-chloro-3-oxobutylthio)ethyl]-N'-cyano-N"-methylguanidineHCID 53629101MethylorthoformateHCID 56924540Ammonium sodium phosphate tetrahydrate

생성물 1

HCID 14457222N-cyano-N'-[2-(3-formylamino-2-oxobutylthio)ethyl]-N"-methylguanidine수율 21%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To 131 mg of N-[2-(2-chloro-3-oxobutylthio)ethyl]-N'-cyano-N"-methylguanidine, 320 mg of ammonium formate, 0.6 ml of methyl orthoformate and 209 mg of sodium ammonium hydrogenphosphate tetrahydrate were added 2.5 ml of formamide and 2.5 ml of chloroform, and the mixture was refluxed for 2 hours. Then, 420 mg of sodium hydrogencarbonate was added to the mixture and the solvent was removed under reduced pressure, and the obtained residue was refined by silica gel column chromatography (developing solvent: ethyl acetate/methanol=10/1) to obtain 28 mg of a colorless oily product (the yield was 21%).

후처리

  1. temperaturethe mixture was refluxed for 2 hours
  2. customthe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-6cbe34cb52e84d88a1fca85832fe3e02
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04886910

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