Ethyl 4-[(2,6-dimethylphenyl)imino]-1-piperidinecarboxylate → HCID 23338990、化合物

HRID 28129ノート

反応式

HRID 28129 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N:9]=[C:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:12][CH2:11]1.[H][H]>[Pt](=O)=O.CO>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[NH:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH2:12][CH2:11]1

参加物

5

反応物 2

HCID 23339012Ethyl 4-[(2,6-dimethylphenyl)imino]-1-piperidinecarboxylateHCID 178418361HCID 178418361、化合物

生成物 1

HCID 23338990HCID 23338990、化合物

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 887Methanol溶媒

実験手順

A mixture of 45 parts of ethyl 4-[(2,6-dimethylphenyl)-imino]-1-piperidinecarboxylate, 0.3 parts of platinum dioxide in 160 parts of methanol is hydrogenated at normal pressure and at a temperature between 24°and 35° C. After the calculated amount of hydrogen is taken up, hydrogenation is stopped. The catalyst is filtered off and the filtrate is evaporated. The oily residue is distilled, to yield 30 parts of the oily free base of ethyl 4-[(2,6-dimethylphenyl)amino]-1-piperidinecarboxylate; bp. 148°-153° C. at 0.01 mm. pressure. From this distillate, the hydrochloride salt is prepared in the usual manner in 1,1'-oxybisethane. The precipitated solid salt is filtered off and dried, yielding 28.5 parts of ethyl 4-[(2,6-dimethylphenyl)amino]-piperidinecarboxylate hydrochloride; mp. 195.5° C.

後処理

  1. customis hydrogenated at normal pressure and at a temperature between 24°and 35° C
  2. filtrationThe catalyst is filtered off
  3. customthe filtrate is evaporated
  4. distillationThe oily residue is distilled

出典と根拠

ORDレコード
ord-8dbfba94f6d545ee8f3f3730a32c8d3b
出典データセット
uspto-grants-1980_09
特許番号
US04225606

反応ノート

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