Potassium Carbonate → 2-Mercapto-6-(3,4-dimethoxyphenyl)-4-methyl-pyridine-3-carbonitrile

HRID 556404

反応式

HRID 556404 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11](=O)[CH2:12][C:13](=O)[CH3:14])[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].[C:17]([CH2:19][C:20]([NH2:22])=[S:21])#[N:18].C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[SH:21][C:20]1[C:19]([C:17]#[N:18])=[C:13]([CH3:14])[CH:12]=[C:11]([C:5]2[CH:6]=[CH:7][C:8]([O:9][CH3:10])=[C:3]([O:2][CH3:1])[CH:4]=2)[N:22]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 3680601-(3,4-Dimethoxyphenyl)butane-1,3-dioneHCID 14162772-Cyanoethanethioamide

生成物 1

HCID 1784885622-Mercapto-6-(3,4-dimethoxyphenyl)-4-methyl-pyridine-3-carbonitrile収率 98.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

5.0 g (22.5 mmol) 1-(3,4-dimethoxyphenyl)butane-1,3-dione, 2.9 g (29.2 mmol) cyanthioacetamide and 4.0 g (29.2 mmol) potassium carbonate are added by stirring to 170 ml acetone at room temperature for 21 h. Then, the solvent is removed and the residue is just dissolved in ethanol/water (1:1). Following acidification with glacial acetic acid, the resulting precipitate is sucked off, washed with some water, suck dried and dried in vacuo at 50° C. 6.34 g (98%) 2-mercapto-6-(3,4-dimethoxyphenyl)-4-methyl-pyridine-3-carbonitrile is obtained.

後処理

  1. customThen, the solvent is removed
  2. dissolutionthe residue is just dissolved in ethanol/water (1:1)
  3. washwashed with some water, suck
  4. customdried
  5. customdried in vacuo at 50° C

出典と根拠

ORDレコード
ord-c19656c7d9f34cc5a27608dd7eb91648
出典データセット
uspto-grants-2011_11
特許番号
US08058285B2

関連ノート

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