2,2,2-Trifluoroethanol → Pyridine, 3-methoxy-2-methyl-4-(2,2,2-trifluoroethoxy)-, 1-oxide

HRID 2258302

反応式

HRID 2258302 の反応式
CC(C)([O-])C.[K+].[CH2:7]([OH:12])[C:8]([F:11])([F:10])[F:9].[CH3:13][C:14]1[C:19]([O:20][CH3:21])=[C:18](Cl)[CH:17]=[CH:16][N+:15]=1[O-:23]>O>[CH3:13][C:14]1[C:19]([O:20][CH3:21])=[C:18]([O:12][CH2:7][C:8]([F:11])([F:10])[F:9])[CH:17]=[CH:16][N+:15]=1[O-:23]

参加物

5

反応物 3

HCID 64092,2,2-TrifluoroethanolHCID 5083929Pyridine, 4-chloro-3-methoxy-2-methyl-, 1-oxideHCID 23665647Potassium tert-butoxide2 回

生成物 1

HCID 14402953Pyridine, 3-methoxy-2-methyl-4-(2,2,2-trifluoroethoxy)-, 1-oxide

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

6.7 g of potassium tert-butoxide were added in portions, at -20° C., while stirring and under a nitrogen atmosphere, 5 to 20 ml of trifluoroethanol. After the mixture had been warmed to 0° C., 5.2 g (30 mmol) of 2-methyl-3-methoxy-4-chloropyridine N-oxide were added in portions. The mixture was heated under reflux for 3 hours, and then left to cool down to room temperature; a further 3.45 g of potassium tert-butoxide were then added and the mixture was heated under reflux for 2 hours. After it had cooled down, 40 ml of water were added to the reaction mixture, which was then extracted with dichloromethane; the extract was then dried over MgSO4 and freed from the solvent in vacuo. The resulting oily product was subjected to further reaction.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 3 hours
  3. waitleft
  4. temperatureto cool down to room temperature
  5. temperaturethe mixture was heated
  6. temperatureunder reflux for 2 hours
  7. temperatureAfter it had cooled down
  8. extractionwas then extracted with dichloromethane
  9. dry with materialthe extract was then dried over MgSO4
  10. customThe resulting oily product was subjected to further reaction

出典と根拠

ORDレコード
ord-6da0327bc5974c779ac08df838b8c9f5
出典データセット
uspto-grants-1997_08
特許番号
US05658933

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