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

반응식

HRID 57658 반응식
[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]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 674017084-(4-(Chloromethyl)phenyl)pyridineHCID 178481352HCID 178481352, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-7cefa2a4d7e740288cdf381fd129b57c
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434730B2

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