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

HRID 260519

反応式

HRID 260519 の反応式
[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

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 215082,3-DibromobutaneHCID 178481768HCID 178481768、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2f37cf315c344f1a8a4df1cb3158c984
出典データセット
uspto-grants-1996_06
特許番号
US05527908

関連ノート

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