Sodium Carbonate → 1-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl}-N-methylaminoacetyl}-4-phenoxypiperidine

HRID 463310노트

반응식

HRID 463310 반응식
Cl.CO.C(O)(=O)C(O)=O.[F:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2([CH2:22][CH2:23][CH2:24][N:25]([CH2:27][C:28]([N:30]3[CH2:35][CH2:34][CH:33]([O:36][C:37]4[CH:42]=[CH:41][CH:40]=[C:39](Cl)[CH:38]=4)[CH2:32][CH2:31]3)=[O:29])[CH3:26])[O:21][CH2:20][CH2:19][O:18]2)=[CH:13][CH:12]=1.[H][H].C(=O)([O-])[O-].[Na+].[Na+]>[Pd].CO>[F:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2([CH2:22][CH2:23][CH2:24][N:25]([CH2:27][C:28]([N:30]3[CH2:31][CH2:32][CH:33]([O:36][C:37]4[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=4)[CH2:34][CH2:35]3)=[O:29])[CH3:26])[O:18][CH2:19][CH2:20][O:21]2)=[CH:13][CH:12]=1

참가 물질

7

반응물 4

HCID 10340Sodium CarbonateHCID 202831291-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl}-N-methylaminoacetyl}-4-(3-chlorophenoxy)piperidine oxalateHCID 21893726Hydrochloride methanolHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 202831171-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl}-N-methylaminoacetyl}-4-phenoxypiperidine

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A suspension prepared from 2.25 g of 5% palladium on carbon, 400 ml of methanol, 0.2 ml of saturated HCl/methanol and 11.19 g (19.3 mmol) of 1-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl}-N-methylaminoacetyl}-4-(3-chlorophenoxy)piperidine oxalate was shaken under 50 psi hydrogen at 50° for 4 hours. The mixture was allowed to cool to room temperature and filtered, and the solvent was evaporated to provide an oil. The oil was shaken with saturated sodium carbonate, extracted with ether, dried over potassium carbonate, filtered, and the solvent evaporated to provide 1-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]-propyl}-N-methylaminoacetyl}-4-phenoxypiperidine.

후처리

  1. filtrationfiltered
  2. customthe solvent was evaporated
  3. customto provide an oil
  4. extractionextracted with ether
  5. dry with materialdried over potassium carbonate
  6. filtrationfiltered
  7. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-51b17dd9911a4565b4e424e5ac0c3315
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04518713

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