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

HRID 2049352노트

반응식

HRID 2049352 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 23338990HCID 23338990, 화합물

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 887Methanol용매

실험 절차

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]-1-piperidinecarboxylate hydrochloride; mp. 195.5° C.

후처리

  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

출처 및 근거

ORD 기록
ord-1d422df6e2bc4f2da8b1b36fe7a71283
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04197304

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