Water → N-cyano-N'-[2-(2,2-dichloro-3-oxobutylthio)]ethyl-N"-methylguanidine

HRID 477274노트

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HRID 477274 반응식
[Cl:1][CH:2]([C:14](=[O:16])[CH3:15])[CH2:3][S:4][CH2:5][CH2:6][NH:7][C:8]([NH:11][C:12]#[N:13])=[N:9][CH3:10].O.[Cl:18]OC(C)(C)C.C(OCC)(=O)C>CO>[C:12]([NH:11][C:8]([NH:7][CH2:6][CH2:5][S:4][CH2:3][C:2]([Cl:18])([Cl:1])[C:14](=[O:16])[CH3:15])=[N:9][CH3:10])#[N:13]

참가 물질

6

반응물 4

HCID 962Water2회HCID 8857Ethyl AcetateHCID 521297Tert-Butyl hypochloriteHCID 14153741N-[2-(2-chloro-3-oxobutylthio)ethyl]-N'-cyano-N"-methylguanidine

생성물 1

HCID 14622765N-cyano-N'-[2-(2,2-dichloro-3-oxobutylthio)]ethyl-N"-methylguanidine수율 16.2%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
0 °C

실험 절차

In 1 ml of methanol was dissolved 131 mg of N-[2-(2-chloro-3-oxobutylthio)]ethyl-N'-cyano-N"-methyl-guanidine, and the solution was cooled with water and 55 mg of t-butyl hypochlorite was added to the solution. The mixture was stirred at 0° C. for 1 hour and 1 ml of water and 15 ml of ethyl acetate were added to the reaction mixture. The ethyl acetate layer was recovered, dried with anhydrous sodium sulfate and concentrated under reduced pressure. The obtained residue was refined by silica gel column chromatography (developing solvent: ethyl acetate/ethanol=10/1) to obtain 24 mg of a colorless oily product (the yield was 16%).

후처리

  1. additionwas added to the solution
  2. customThe ethyl acetate layer was recovered
  3. dry with materialdried with anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-82ebaf3da70f4305a87a9ad7daedea54
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04886912

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