Potassium Carbonate → 5-methyl-7-neopentyl-2-(4-(pyridin-4-yl)benzyl)-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione

HRID 57658

反応式

HRID 57658 の反応式
[CH3:1][N:2]1[C:7](=[O:8])[C:6]2=[CH:9][NH:10][N:11]=[C:5]2[N:4]([CH2:12][C:13]([CH3:16])([CH3:15])[CH3:14])[C:3]1=[O:17].Cl[CH2:19][C:20]1[CH:25]=[CH:24][C:23]([C:26]2[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=2)=[CH:22][CH:21]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[CH3:1][N:2]1[C:7](=[O:8])[C:6]2=[CH:9][N:10]([CH2:19][C:20]3[CH:21]=[CH:22][C:23]([C:26]4[CH:31]=[CH:30][N:29]=[CH:28][CH:27]=4)=[CH:24][CH:25]=3)[N:11]=[C:5]2[N:4]([CH2:12][C:13]([CH3:14])([CH3:16])[CH3:15])[C:3]1=[O:17]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 674017084-(4-(Chloromethyl)phenyl)pyridineHCID 178481352HCID 178481352、化合物

生成物 1

HCID 700974725-methyl-7-neopentyl-2-(4-(pyridin-4-yl)benzyl)-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione収率 126.4%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

5-methyl-7-neopentyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (236 mg, 1.0 mmol), 4-(4-(chloromethyl)phenyl)pyridine (305 mg, 1.5 mmol) and potassium carbonate (414 mg, 3.0 mmol) are suspensed in 3 mL of DMF. The reaction mixture is stirred at room temperature overnight, and then diluted with 100 mL of water. The mixture is extracted with methylene chloride four times (40 mL×4). The combined organic phase is dried over anhydrous sodium sulfate. After filtration, the filtrate is evaporated to dryness to give 510 mg of crude product, which is used in the next step without further purification. MS (ESI) m/z 404.2 [M+H]+.

後処理

  1. extractionThe mixture is extracted with methylene chloride four times (40 mL×4)
  2. dry with materialThe combined organic phase is dried over anhydrous sodium sulfate
  3. filtrationAfter filtration
  4. customthe filtrate is evaporated to dryness

出典と根拠

ORDレコード
ord-7cefa2a4d7e740288cdf381fd129b57c
出典データセット
uspto-grants-2016_09
特許番号
US09434730B2

関連ノート

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