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Hydrochloric Acid → 1-{2-{N-[4-(4-Fluorophenyl)-4-oxobutyl]-N-ethylamino}ethyl}-4-(3-chlorophenoxy)piperidine dihydrochloride

HRID 463314
ノート
印刷プレビュー

反応式

HRID 463314 の反応式
[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]([CH2:21][CH2:22][N:23]3[CH2:28][CH2:27][CH:26]([O:29][C:30]4[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[CH:31]=4)[CH2:25][CH2:24]3)[CH2:19][CH3:20])OCC[O:11]2)=[CH:6][CH:5]=1.Cl.C(=O)(O)[O-].[Na+].C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl>CO>[ClH:36].[ClH:1].[F:3][C:4]1[CH:9]=[CH:8][C:7]([C:10](=[O:11])[CH2:15][CH2:16][CH2:17][N:18]([CH2:21][CH2:22][N:23]2[CH2:24][CH2:25][CH:26]([O:29][C:30]3[CH:35]=[CH:34][CH:33]=[C:32]([Cl:36])[CH:31]=3)[CH2:27][CH2:28]2)[CH2:19][CH3:20])=[CH:6][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 516892Sodium BicarbonateHCID 20283085HCID 20283085、化合物

生成物 1

HCID 202831201-{2-{N-[4-(4-Fluorophenyl)-4-oxobutyl]-N-ethylamino}ethyl}-4-(3-chlorophenoxy)piperidine dihydrochloride

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒
2 回

実験手順

A solution of 5.68 g (10.1 mmol) of 1-{2-{N-{3-[2-(4-fluorophenyl)-1,3-dioxolan-2-yl]propyl}-N-ethylamino}ethyl}-4-(3-chlorophenoxy)piperidine dihydrochloride, 150 ml of methanol and 70 ml of 3N HCl was heated at reflux for 4 hours under nitrogen and allowed to cool to room temperature. The mixture was neutralized with saturated sodium bicarbonate after which the methanol was evaporated. The residual aqueous solution was made basic with saturated sodium carbonate, extracted twice with ether and dried over potassium carbonate. Evaporation of the solvent provided an oil. The yield of the dihydrochloride was 5.20 g (99%). Recrystallization from ethanol provided 4.16 g (80%) of analytically pure material.

後処理

  1. temperatureat reflux for 4 hours under nitrogen
  2. customwas evaporated
  3. extractionextracted twice with ether
  4. dry with materialdried over potassium carbonate
  5. customEvaporation of the solvent
  6. customprovided an oil
  7. customRecrystallization from ethanol
  8. customprovided 4.16 g (80%) of analytically pure material

出典と根拠

ORDレコード
ord-d7caedbd238749b7951d73ccc137b3bc
出典データセット
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04518713

反応ノート

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