Sodium → 5-Propyl-2-(4-trifluoromethylphenyl)pyrimidine

HRID 1788641ノート

反応式

HRID 1788641 の反応式
Cl.[F:2][C:3]([F:14])([F:13])[C:4]1[CH:12]=[CH:11][C:7]([C:8]([NH2:10])=[NH:9])=[CH:6][CH:5]=1.C[O-].[Na+].[Na]>CO>[CH2:5]([C:4]1[CH:3]=[N:9][C:8]([C:7]2[CH:11]=[CH:12][C:4]([C:3]([F:13])([F:14])[F:2])=[CH:5][CH:6]=2)=[N:10][CH:12]=1)[CH2:6][CH3:7]

参加物

5

反応物 3

HCID 5360545SodiumHCID 10942334Sodium MethoxideHCID 125357914-(Trifluoromethyl)benzamidine Hydrochloride

生成物 1

HCID 139315715-Propyl-2-(4-trifluoromethylphenyl)pyrimidine収率 100%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4-Trifluoromethylbenzamidine hydrochloride (5 g, 0.02 mol) and α-propyl-β-dimethylaminoacrolein (3 g, 0.02 mol) were added to a sodium methylate solution having metallic sodium (1 g) dissolved in anhydrous methanol (50 ml), followed by boiling the mixture for 4 hours with stirring, distilling off methanol, adding toluene (50 ml) to the reaction residue to extract the product, washing the resulting extract with water, drying the toluene layer with anhydrous sodium sulfate, distilling off toulene and three times recrystallizing the residue from methanol to obtain 5-propyl-2-(4-trifluoromethylphenyl)pyrimidine (3 g, 0.01 mol).

後処理

  1. customfor 4 hours
  2. distillationdistilling off methanol
  3. additionadding toluene (50 ml) to the reaction residue
  4. extractionto extract the product
  5. washwashing the resulting
  6. extractionextract with water
  7. dry with materialdrying the toluene layer with anhydrous sodium sulfate
  8. distillationdistilling off toulene and three times
  9. customrecrystallizing the residue from methanol

出典と根拠

ORDレコード
ord-a5ca049c5eda4598a16a6e6dcc623604
出典データセット
uspto-grants-1987_08
特許番号
US04684476

反応ノート

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