Hydrochloric Acid → 1-{2-{N-[4-(4-Fluorophenyl)-4-oxobutyl]-N-methylamino}ethyl}-4-(4-chlorophenoxy)piperidine dihydrochloride

HRID 463323노트

반응식

HRID 463323 반응식
[ClH:1].Cl.[F:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2([CH2:15][CH2:16][CH2:17][N:18]([CH2:20][CH2:21][N:22]3[CH2:27][CH2:26][CH:25]([O:28][C:29]4[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][CH:30]=4)[CH2:24][CH2:23]3)[CH3:19])OCC[O:11]2)=[CH:6][CH:5]=1.Cl.C(=O)([O-])[O-].[Na+].[Na+].C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl>CO>[ClH:35].[ClH:1].[F:3][C:4]1[CH:5]=[CH:6][C:7]([C:10](=[O:11])[CH2:15][CH2:16][CH2:17][N:18]([CH2:20][CH2:21][N:22]2[CH2:23][CH2:24][CH:25]([O:28][C:29]3[CH:34]=[CH:33][C:32]([Cl:35])=[CH:31][CH:30]=3)[CH2:26][CH2:27]2)[CH3:19])=[CH:8][CH:9]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 20283107HCID 20283107, 화합물

생성물 1

HCID 202830801-{2-{N-[4-(4-Fluorophenyl)-4-oxobutyl]-N-methylamino}ethyl}-4-(4-chlorophenoxy)piperidine dihydrochloride수율 52.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 8.94 g (17.7 mmol) of 1-{2-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl}-N-methylamino}ethyl}-4-(4-chlorophenoxy)piperidine dihydrochloride, 135 ml of methanol, and 55 ml of 3N HCl was heated at reflux for 3 hours under nitrogen. The mixture was allowed to cool to room temperature, poured into saturated sodium carbonate, extracted twice with ether and dried over potassium carbonate. Filtration followed by evaporation of the solvent provided an oil. The yield of a crude dihydrochloride was 6.71 g (81%). Recrystallization from ethanol provided 2.37 g (28%) of the desired ketone.

후처리

  1. temperatureat reflux for 3 hours under nitrogen
  2. extractionextracted twice with ether
  3. dry with materialdried over potassium carbonate
  4. filtrationFiltration
  5. customfollowed by evaporation of the solvent
  6. customprovided an oil
  7. customRecrystallization from ethanol

출처 및 근거

ORD 기록
ord-4e55e6e76f4440a19cf54d9609105e0e
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04518713

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