Hydrochloric Acid → 4-Benzyl-1-[2-(4-hydroxy-phenoxy)-ethyl]-piperidin-4-ol hydrochloride

HRID 1419892ノート

反応式

HRID 1419892 の反応式
[CH2:1]([C:8]1([OH:31])[CH2:13][CH2:12][N:11]([CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][C:20]([O:23]CC3C=CC=CC=3)=[CH:19][CH:18]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[ClH:32]>CO.C(OCC)(=O)C.[Pd]>[ClH:32].[CH2:1]([C:8]1([OH:31])[CH2:9][CH2:10][N:11]([CH2:14][CH2:15][O:16][C:17]2[CH:22]=[CH:21][C:20]([OH:23])=[CH:19][CH:18]=2)[CH2:12][CH2:13]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 700459094-Benzyl-1-[2-(4-benzyloxy-phenoxy)-ethyl]-piperidin-4-ol

生成物 1

HCID 232944494-Benzyl-1-[2-(4-hydroxy-phenoxy)-ethyl]-piperidin-4-ol hydrochloride収率 72%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒HCID 23938Palladium溶媒

実験手順

4-Benzyl-1-[2-(4-benzyloxy-phenoxy)-ethyl]-piperidin-4-ol (1.35 g, 3.2 mmol) was dissolved in a mixture of MeOH (75 ml) and ethyl acetate (75 ml) and hydrogenated in the presence of Pd on C at room temperature and atmospheric pressure. After filtration and evaporation of the solvent, the residue was dissolved in ethanol (2 mnl) and ethyl acetate (10 ml). 1.1 equivalent of ethanolic HCl were added to give 4-benzyl-1-[2-(4-hydroxy-phenoxy)-ethyl]-piperidin-4-ol hydrochloride (0.85 g, 72%) as colorless solid, m.p. 161°-163° C. and MS: m/e=328.3 (M+H+).

後処理

  1. filtrationAfter filtration and evaporation of the solvent
  2. dissolutionthe residue was dissolved in ethanol (2 mnl)

出典と根拠

ORDレコード
ord-63c2fc9015a34f9394b7b010ffbb963a
出典データセット
uspto-grants-1999_03
特許番号
US05889026

反応ノート

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