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

HRID 463310ノート

反応式

HRID 463310 の反応式
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

参加物

7

反応物 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、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-51b17dd9911a4565b4e424e5ac0c3315
出典データセット
uspto-grants-1985_05
特許番号
US04518713

反応ノート

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