Water → HCID 86723474, 화합물

HRID 2201239노트

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HRID 2201239 반응식
[CH3:1][N:2]1[C:7]2=[CH:8][NH:9][C:10]([C:11]3[CH:15]=[CH:14][N:13]([CH3:16])[N:12]=3)=[C:6]2[C:5](=[O:17])[N:4]([CH3:18])[C:3]1=[O:19].Br[CH2:21][CH2:22][CH2:23][C:24]([N:26]([O:28][CH3:29])[CH3:27])=[O:25].C(=O)([O-])[O-].[Cs+].[Cs+].O>CN(C=O)C>[CH3:1][N:2]1[C:7]2=[CH:8][N:9]([CH2:21][CH2:22][CH2:23][C:24]([N:26]([O:28][CH3:29])[CH3:27])=[O:25])[C:10]([C:11]3[CH:15]=[CH:14][N:13]([CH3:16])[N:12]=3)=[C:6]2[C:5](=[O:17])[N:4]([CH3:18])[C:3]1=[O:19]

참가 물질

6

반응물 4

HCID 962WaterHCID 10796Cesium carbonateHCID 14642623130250-57-62회HCID 1363484071,3-Dimethyl-5-(1-methyl-1H-pyrazol-3-yl)-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione

생성물 1

HCID 86723474HCID 86723474, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1,3-Dimethyl-5-(1-methyl-1H-pyrazol-3-yl)-1H-pyrrolo[3,4-d]pyrimidine-2,4(3H,6H)-dione (800 mg, 3.09 mmol), 4-bromo-N-methoxy-N-methylbutanamide (Intermediate P) (843 mg, 4.01 mmol) and cesium carbonate (2011 mg, 6.17 mmol) were suspended in DMF (11.100 ml) and the mixture was stirred at room temperature for 22 hours. The mixture was poured into water (50 ml) and extracted with DCM (3×100 ml). The combined organic extracts were washed with water (2×50 ml) and brine (50 ml), dried over sodium sulfate and evaporated under vacuum. Purification by mass-directed HPLC under the following conditions afforded the title compound.

후처리

  1. extractionextracted with DCM (3×100 ml)
  2. washThe combined organic extracts were washed with water (2×50 ml) and brine (50 ml)
  3. dry with materialdried over sodium sulfate
  4. customevaporated under vacuum
  5. customPurification by mass-directed HPLC under the following conditions

출처 및 근거

ORD 기록
ord-514708b0248943feaf8185d1a94909ed
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09359381B2

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