Cesium carbonate → HCID 19805500, 화합물

HRID 1681697

반응식

HRID 1681697 반응식
Cl[CH2:2][C:3]1[N:4]([CH3:8])[CH:5]=[CH:6][N:7]=1.[C:9]([N:14]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16](=[O:23])[NH:15]1)([O:11][CH2:12][CH3:13])=[O:10].C(=O)([O-])[O-].[Cs+].[Cs+]>CN(C)C=O>[C:9]([N:14]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16](=[O:23])[N:15]1[CH2:2][C:3]1[N:4]([CH3:8])[CH:5]=[CH:6][N:7]=1)([O:11][CH2:12][CH3:13])=[O:10]

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 584113Ethyl 3-oxo-2,3-dihydro-1H-indazole-1-carboxylateHCID 7365362-(chloromethyl)-1-methyl-1H-imidazole

생성물 1

HCID 19805500HCID 19805500, 화합물수율 67%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

2-Chloromethyl-1-methylimidazole (0.91 g) was added portionwise to a stirred mixture of 1,2-dihydro-1-carboethoxy-3H-indazol-3-one (1.03 g), caesium carbonate (5.4 g) and N,N-dimethylformamide (DMF, 5 ml). The mixture was heated to 80° C. for 4 hours under an atmosphere of argon, cooled to ambient temperature and filtered. The filtrate was diluted with water and extracted with ethyl acetate. The solid was washed with ethyl acetate. The organic solutions were combined, washed with a saturated aqueous sodium chloride solution, dried (MgSO4) and evaporated. The oil residue crystallised on trituration under diethyl ether. There was thus obtained a mixture (1 g, 67% of 1,2-dihydro-1-carboethoxy-2-(1-methylimidazol-2-yl)methyl-3H-indazol-3-one and 1-carboethoxy-3-(1-methylimidazol-2-yl)methoxy-1H-indazole (starting material for Ex. 145).

후처리

  1. temperaturecooled to ambient temperature
  2. filtrationfiltered
  3. additionThe filtrate was diluted with water
  4. extractionextracted with ethyl acetate
  5. washThe solid was washed with ethyl acetate
  6. washwashed with a saturated aqueous sodium chloride solution
  7. dry with materialdried (MgSO4)
  8. customevaporated
  9. customThe oil residue crystallised on trituration under diethyl ether

출처 및 근거

ORD 기록
ord-88a00675ace7406b80429698b46d43a3
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05173496

연결된 노트

불러오는 중…