Cesium carbonate → HCID 136304034, 화합물

HRID 1409326노트

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HRID 1409326 반응식
[O:1]=[C:2]1[N:7]2[CH:8]=[C:9]([C:11]([O:13]CC)=[O:12])[N:10]=[C:6]2[CH:5]=[CH:4][NH:3]1.C(=O)([O-])[O-].[Cs+].[Cs+]>C(O)C.O>[O:1]=[C:2]1[N:7]2[CH:8]=[C:9]([C:11]([OH:13])=[O:12])[N:10]=[C:6]2[CH:5]=[CH:4][NH:3]1

참가 물질

5

실험 절차

Ethyl 5-oxo-5,6-dihydroimidazo[1,2-c]pyrimidine-2-carboxylate (2.510 mmol, 0.52 g) was suspended in ethanol (20 ml). Cesium carbonate (5.02 mmol, 1.635 g) dissolved in water (4 ml) was added and the resulting mixture was stirred at RT for 3.5 h after which the mixture was refluxed for 8 h. The ethanol was evaporated, and the residue was diluted with water. The pH was adjusted to 4 with 1 M HCl and the solvent was evaporated. The residue was purified by trituration from DMF. 0.137 g of the title compound was obtained. 1H-NMR (400 MHz, CDCl3): δ 7.17-7.31 (m, 2H), 7.86-7.99 (m, 1H).

후처리

  1. additionwas added
  2. temperaturewas refluxed for 8 h
  3. customThe ethanol was evaporated
  4. additionthe residue was diluted with water
  5. customthe solvent was evaporated
  6. customThe residue was purified by trituration from DMF

출처 및 근거

ORD 기록
ord-05957157090a46ac96547bc412afa171
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08921378B2

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