Ethanol → HCID 178517000、化合物

HRID 1263962

反応式

HRID 1263962 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 178517000HCID 178517000、化合物収率 71%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-745387b526604d45aedc416250d6ef80
出典データセット
uspto-grants-2003_04
特許番号
US06541503B2

関連ノート

読み込み中…