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

HRID 1788641노트

반응식

HRID 1788641 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 139315715-Propyl-2-(4-trifluoromethylphenyl)pyrimidine수율 100%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-a5ca049c5eda4598a16a6e6dcc623604
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04684476

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