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

HRID 477273ノート

反応式

HRID 477273 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-959a54c27c094801bf58b2dfebe9a1fd
出典データセット
uspto-grants-1989_12
特許番号
US04886912

反応ノート

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