Ethanol → HCID 178517000, 화합물

HRID 1263962

반응식

HRID 1263962 반응식
C(O[CH:4]=[C:5]1[C:16]2[C:8](=[CH:9][CH:10]=[C:11]3[C:15]=2[S:14][CH:13]=[N:12]3)[NH:7][C:6]1=[O:17])C.[CH:18]1[CH:19]=[CH:20][N:21]=[C:22]([NH:24][S:25]([C:28]2[CH:29]=[CH:30][C:31]([NH2:34])=[CH:32][CH:33]=2)(=[O:27])=[O:26])[CH:23]=1.C(O)C>O>[O:17]=[C:6]1[C:5](=[CH:4][NH:34][C:31]2[CH:30]=[CH:29][C:28]([S:25]([NH:24][C:22]3[CH:23]=[CH:18][CH:19]=[CH:20][N:21]=3)(=[O:27])=[O:26])=[CH:33][CH:32]=2)[C:16]2[C:8](=[CH:9][CH:10]=[C:11]3[C:15]=2[S:14][CH:13]=[N:12]3)[NH:7]1

참가 물질

5

반응물 3

HCID 702EthanolHCID 5336SulfapyridineHCID 539908078-[Ethoxymethylidene]-6H-[1,3]thiazolo[5,4-e]indol-7-one

생성물 1

HCID 178517000HCID 178517000, 화합물수율 71%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a 25 ml round bottom flask was added a stir bar, 246 mg (1.00 mmol) of 8-ethoxymethylene-6,8-dihydro-1-thia-3,6-diaza-as-indacen-7-one. 249 (1.00 mmol) of sulfapyridine and 10 ml of ethanol. The flask was fitted with a water-cooled reflux condenser, and the mixture was heated to reflux using an oil bath with stirring for 18 h. The reaction was allowed to cool and was filtered. The precipitate was washed with excess ethanol and dried under vacuum to yield 321 mg (71%) of the title compound: 1H NMR (DMSO-d6): δ 11.9 (br s, 1H), 11.2 (d, 1H), 10.9 (s, 1H), 9.3 (s, 1H), 8.1 (d, 2H), 7.9 (m 3H) 7.8 (m, 1H), 7.6 (d, 2H), 7.2 (d, 1H), 7.2 (d, 1H), 6.9 (t, 1H); C21H15N5O3S2: APCI−MS m/z 450 (M+H)+.

후처리

  1. additionTo a 25 ml round bottom flask was added a stir bar
  2. temperaturecooled
  3. temperaturereflux condenser
  4. temperaturethe mixture was heated
  5. temperatureto reflux
  6. temperatureto cool
  7. filtrationwas filtered
  8. washThe precipitate was washed with excess ethanol
  9. customdried under vacuum

출처 및 근거

ORD 기록
ord-745387b526604d45aedc416250d6ef80
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06541503B2

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