Methyl 2-cyano-3,3-bis(methylsulfanyl)prop-2-enoate → HCID 178503357、化合物

HRID 624816

反応式

HRID 624816 の反応式
C[O:2][C:3](=O)[C:4]([C:10]#[N:11])=[C:5](SC)[S:6][CH3:7].[NH2:13][C:14]1[CH:18]=[CH:17][NH:16][N:15]=1>C(O)C>[OH:2][C:3]1[N:15]2[N:16]=[CH:17][CH:18]=[C:14]2[N:13]=[C:5]([S:6][CH3:7])[C:4]=1[C:10]#[N:11]

参加物

4

反応物 2

HCID 319957Methyl 2-cyano-3,3-bis(methylsulfanyl)prop-2-enoateHCID 178418806HCID 178418806、化合物

生成物 1

HCID 178503357HCID 178503357、化合物収率 67%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Under nitrogen gas atmosphere, 2-cyano-3,3-bismethylthio-2-propenoic methyl ester (6 g, 29.5 mmol) was added to ethanol (40 mL) along with 3-aminopyrazole (2.6 g, 31 mmol) and the mixture was refluxed for 2.5 hours. The reaction was then cooled to room temperature and precipitate was collected by filtration under vacuum. The solid was washed with ethanol and dried under vacuum to give 7-hydroxy-5-(methylthio)pyrazolo[1,5-a]pyrimidine-6-carbonitrile in 67% yield (4.1 g). This material was used for the next step without further purification. LCMS (M+1=207)

後処理

  1. temperaturethe mixture was refluxed for 2.5 hours
  2. filtrationprecipitate was collected by filtration under vacuum
  3. washThe solid was washed with ethanol
  4. customdried under vacuum

出典と根拠

ORDレコード
ord-42f1683331804e74b76cc2792bba2865
出典データセット
uspto-grants-2016_04
特許番号
US09303033B2

関連ノート

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