Ethanol → Ethyl 1-benzyl-4-hydroxypiperidine-4-carboxylate

HRID 1085722ノート

反応式

HRID 1085722 の反応式
S(=O)(=O)(O)O.Cl.[CH2:7]([N:14]1[CH2:19][CH2:18][C:17]([C:21]#N)([OH:20])[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.C(=O)([O-])[OH:24].[Na+].[CH2:28]([OH:30])[CH3:29]>>[CH2:7]([N:14]1[CH2:19][CH2:18][C:17]([C:21]([O:30][CH2:28][CH3:29])=[O:24])([OH:20])[CH2:16][CH2:15]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

5

反応物 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 27237801-Benzyl-4-hydroxypiperidine-4-carbonitrile monohydrochloride

生成物 1

HCID 272010Ethyl 1-benzyl-4-hydroxypiperidine-4-carboxylate

反応条件

温度
130 °C

実験手順

Conc. sulfuric acid (12 ml) was added to an ethanol solution (50 ml) of 1-benzyl-4-cyano-4-hydroxypiperidine hydrochloride (10 g) and the resulting mixture was heated at 130° C. for 24 hours in a sealed tube. After concentration of the reaction mixture, ice water was added to the concentrate. The resulting mixture was added with an aqueous solution of sodium hydrogencarbonate. After adjusting the thus-obtained solution to pH 7.0, it was extracted with diethyl ether. The extract was washed with brine and then added with anhydrous sodium sulfate to dry the same. The solvent was distilled off to obtain the intended product (9.7 g).

後処理

  1. extractionwas extracted with diethyl ether
  2. washThe extract was washed with brine
  3. additionadded with anhydrous sodium sulfate
  4. customto dry the same
  5. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-edcb30e474d14f59a19d8f2a61af3835
出典データセット
uspto-grants-1991_04
特許番号
US05010188

反応ノート

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