Acetic Acid → 1-(Piperidine-4-yl)-2-ethyl-5-fluoro-1H-indole

HRID 1984984노트

반응식

HRID 1984984 반응식
C([N:8]1[CH2:13][CH2:12][CH:11]([N:14]2[C:22]3[C:17](=[CH:18][C:19]([F:23])=[CH:20][CH:21]=3)[CH:16]=[C:15]2[CH2:24][CH3:25])[CH2:10][CH2:9]1)C1C=CC=CC=1.C(O)(=O)C>CO>[NH:8]1[CH2:13][CH2:12][CH:11]([N:14]2[C:22]3[C:17](=[CH:18][C:19]([F:23])=[CH:20][CH:21]=3)[CH:16]=[C:15]2[CH2:24][CH3:25])[CH2:10][CH2:9]1

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 577188391-(1-benzyl-piperidine-4-yl)-2-ethyl-5-fluoro-1H-indole

생성물 1

HCID 577188301-(Piperidine-4-yl)-2-ethyl-5-fluoro-1H-indole수율 73.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 1-(1-benzyl-piperidine-4-yl)-2-ethyl-5-fluoro-1H-indole (11.9 g) and acetic acid (4.1 ml) in methanol (250 ml) was hydrogenated for 8 h (50° C./1013 mbar). The mixture was then filtered and concentrated in vacuo. CH2Cl2 (250 ml), NaHCO3 (100 ml) and water (300 ml) were added and the mixture stirred for 10 min. The organic layer was extracted with CHCl3 and this was dried (MgSO4) and concentrated in vacuo. 6.4 g of pure product (73%) as colourless crystals was obtained by recrystallisation from ether/petroleum ether.

후처리

  1. custom(50° C./1013 mbar)
  2. filtrationThe mixture was then filtered
  3. concentrationconcentrated in vacuo
  4. additionCH2Cl2 (250 ml), NaHCO3 (100 ml) and water (300 ml) were added
  5. extractionThe organic layer was extracted with CHCl3
  6. dry with materialthis was dried (MgSO4)
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-c0d57c47f2d5440fb83779cc0ebd3055
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07544806B2

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