Potassium Carbonate → HCID 67046696、化合物

HRID 606367ノート

反応式

HRID 606367 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]#[N:10])[CH:5]=[CH:6][CH:7]=1.O.[C:12]([OH:16])(=[O:15])[CH:13]=O.C(=O)([O-])[O-].[K+:21].[K+]>CO>[C:9]([C:8]([C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([CH3:1])[CH:3]=1)=[CH:13][C:12]([O-:16])=[O:15])#[N:10].[K+:21]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 76279m-MethylphenylacetonitrileHCID 15620607Glyoxylic acid, monohydrate

生成物 1

HCID 67046696HCID 67046696、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred solution of (3-methylphenyl)-acetonitrile (21.6 ml, 165 mmol) in methanol (500 ml) were added glyoxylic acid hydrate (22.7 g, 247 mmol) and potassium carbonate (57.0 g, 412 mmol). The reaction mixture was stirred at room temperature for 2 hours followed by 3 hours at reflux. The precipitate was filtered off, washed with methanol (300 ml), dichloromethane (DCM) (300 ml) and then dried under air suction. The desired product was obtained as a white solid which was used in the next step without further purification.

後処理

  1. waitfollowed by 3 hours
  2. temperatureat reflux
  3. filtrationThe precipitate was filtered off
  4. washwashed with methanol (300 ml), dichloromethane (DCM) (300 ml)
  5. customdried under air suction

出典と根拠

ORDレコード
ord-8a49724fa3864666a18aea7e24c2e0b6
出典データセット
uspto-grants-2011_03
特許番号
US07915304B2

反応ノート

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