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

HRID 583063노트

반응식

HRID 583063 반응식
[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

참가 물질

5

반응물 3

HCID 14797Potassium Hydroxide2회HCID 3512786-FluoroindoleHCID 21584170Piperidin-4-one hydrate

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-be80ee73b12a47e0a1bbaa7850f2a575
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05929072

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