1,1,3,3-Tetraethoxy-2-methylpropane → 6-Methyl-2-phenylpyrazolo[1,5-a]pyrimidine

HRID 1924279노트

반응식

HRID 1924279 반응식
[C:1]1([C:7]2[CH:11]=[C:10]([NH2:12])[NH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(O[CH:16](OCC)[CH:17]([CH3:25])[CH:18](OCC)OCC)C>CC(O)=O>[CH3:25][C:17]1[CH:16]=[N:12][C:10]2[N:9]([N:8]=[C:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH:11]=2)[CH:18]=1

참가 물질

4

반응물 2

HCID 827611,1,3,3-Tetraethoxy-2-methylpropaneHCID 1366553-Amino-5-phenylpyrazole

생성물 1

HCID 577430576-Methyl-2-phenylpyrazolo[1,5-a]pyrimidine수율 45%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
100 °C

실험 절차

To a solution of 3-phenyl-1H-pyrazol-5-amine x120 (31.4 mmol, 1 eq, 5 g) in AcOH (30 ml) is added 1,1,3,3-tetraethoxy-2-methylpropane x121 (31.4 mmol, 1 eq, 7.36 g). The mixture is heated at 100° C. during 4 hours. After evaporation of the solvent under reduced pressure, the crude product is poured in saturated NaHCO3 aqueous solution and then extracted with AcOEt. The cumulated organic layers are dried over MgSO4, filtered and evaporated under reduce pressure. The crude mixture is recristallized in AcOEt to afford 6-methyl-2-phenylpyrazolo[1,5-a]pyrimidine x122 as a solid (3 g).

후처리

  1. customAfter evaporation of the solvent under reduced pressure
  2. additionthe crude product is poured in saturated NaHCO3 aqueous solution
  3. extractionextracted with AcOEt
  4. dry with materialThe cumulated organic layers are dried over MgSO4
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-b9d57b768f8743cdbe88e8f9ef4843fe
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08178533B2

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