Potassium Hydroxide → 6-fluoro-3-(1,2,3,6-tetrahydropyridin-4-yl)-1H-indole

HRID 583063ノート

反応式

HRID 583063 の反応式
[OH-].[K+].[F:3][C:4]1[CH:12]=[C:11]2[C:7]([CH:8]=[CH:9][NH:10]2)=[CH:6][CH:5]=1.O.[NH:14]1[CH2:19][CH2:18][C:17](=O)[CH2:16][CH2:15]1>CO>[F:3][C:4]1[CH:12]=[C:11]2[C:7]([C:8]([C:17]3[CH2:18][CH2:19][NH:14][CH2:15][CH:16]=3)=[CH:9][NH:10]2)=[CH:6][CH:5]=1

参加物

5

反応物 3

HCID 14797Potassium Hydroxide2 回HCID 3512786-FluoroindoleHCID 21584170Piperidin-4-one hydrate

生成物 1

HCID 110530726-fluoro-3-(1,2,3,6-tetrahydropyridin-4-yl)-1H-indole

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Powdered potassium hydroxide (144.4 g) was added carefully to a mechanically stirred mixture of 6-fluoroindole (49.23 g, 0.364 mol) and 4-piperidone monohydrate (111.93 g, 0.728 mol) in methanol (1500 ml). The mixture was then heated under reflux under nitrogen for 18 hours and then more potassium hydroxide (40 g) was added and the reaction mixture heated under reflux for a further 4 hours. The reaction mixture was allowed to cool to room temperature and poured onto ice-water (3000 ml) and stirred for 1 hour and the precipitated solid isolated by filtration and dried at 50° C. in vacuo to give a solid.

後処理

  1. temperatureThe mixture was then heated
  2. temperatureunder reflux under nitrogen for 18 hours
  3. temperaturethe reaction mixture heated
  4. temperatureunder reflux for a further 4 hours
  5. additionpoured onto ice-water (3000 ml)
  6. customthe precipitated solid isolated by filtration
  7. customdried at 50° C. in vacuo
  8. customto give a solid

出典と根拠

ORDレコード
ord-be80ee73b12a47e0a1bbaa7850f2a575
出典データセット
uspto-grants-1999_07
特許番号
US05929072

反応ノート

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