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

HRID 477273노트

반응식

HRID 477273 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].[Cl:17][O-].[Na+].C(OCC)(=O)C>CO>[C:12]([NH:11][C:8]([NH:7][CH2:6][CH2:5][S:4][CH2:3][C:2]([Cl:17])([Cl:1])[C:14](=[O:16])[CH3:15])=[N:9][CH3:10])#[N:13]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 14153741N-[2-(2-chloro-3-oxobutylthio)ethyl]-N'-cyano-N"-methylguanidineHCID 23665760Sodium Hypochlorite

생성물 1

HCID 14622765N-cyano-N'-[2-(2,2-dichloro-3-oxobutylthio)]ethyl-N"-methylguanidine수율 25%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In 1 ml of methanol was dissolved 131 mg of N-[2-(2-chloro-3-oxobutylthio)]ethyl-N'-cyano-N"-methylguanidine, and 0.63 ml of an aqueous solution of sodium hypochlorite was added to the solution and reaction was carried out at room temperature for 3 hours. Then, 15 ml of ethyl acetate was added to the reaction liquid and the organic layer was recovered. The obtained organic layer was dried with anhydrous sodium sulfate and concentrated under reduced pressure. The obtained residue was refined by silica gel column chromatography (developing solvent: ethyl/ethanol=10/1) to obtain 37 mg of a colorless oily product (the yield was 25%).

후처리

  1. additionwas added to the solution and reaction
  2. customthe organic layer was recovered
  3. dry with materialThe obtained organic layer was dried with anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-959a54c27c094801bf58b2dfebe9a1fd
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04886912

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