Potassium Carbonate → 6,7-Dihydro-1,6,7-trimethylpyrazolo[3,4-d]thiazolo[3,2-a]pyrimidin-4(1H)-one

HRID 260519

반응식

HRID 260519 반응식
[SH:1][C:2]1[NH:3][C:4](=[O:12])[C:5]2[CH:10]=[N:9][N:8]([CH3:11])[C:6]=2[N:7]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH:20]([CH:22](Br)[CH3:23])[CH3:21]>CN(C)C=O>[CH3:11][N:8]1[C:6]2[N:7]=[C:2]3[S:1][CH:22]([CH3:23])[CH:20]([CH3:21])[N:3]3[C:4](=[O:12])[C:5]=2[CH:10]=[N:9]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 215082,3-DibromobutaneHCID 178481768HCID 178481768, 화합물

생성물 1

HCID 224016736,7-Dihydro-1,6,7-trimethylpyrazolo[3,4-d]thiazolo[3,2-a]pyrimidin-4(1H)-one수율 12.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

In 200 ml of dimethylformamide was dissolved 10.0 g (54.9 mmol) of 4,5-dihydro-6-mercapto-1-methylpyrazolo[3,4-d]pyrimidin-4(1H)-one [Helv. Chim. Acta, 42, 349 (1959)], and 15.2 g (110 mmol) of potassium carbonate and 10.1 ml (82.3 mmol) of 2,3-dibromobutane were added to the solution, followed by stirring at 80° C. for 3 hours. After evaporation of the solvent, the residue was subjected to partition between chloroform and water, and the chloroform layer was concentrated to dryness under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with chloroform to give 1.57 g (12%) of Compound 41. The compound was recrystallized from ethyl acetate/hexane for purification.

후처리

  1. additionwere added to the solution
  2. customAfter evaporation of the solvent
  3. customto partition between chloroform and water
  4. concentrationthe chloroform layer was concentrated to dryness under reduced pressure
  5. washeluted with chloroform

출처 및 근거

ORD 기록
ord-2f37cf315c344f1a8a4df1cb3158c984
출처 데이터셋
uspto-grants-1996_06
특허 번호
US05527908

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