Pyridine → HCID 23339068, 화합물

HRID 28134노트

반응식

HRID 28134 반응식
[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.N1C=CC=CC=1.[C:27]1([CH2:33][C:34](Cl)=[O:35])[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1>C1C=CC=CC=1>[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[N: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)[C:34](=[O:35])[CH2:33][C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1

참가 물질

5

반응물 3

HCID 1049PyridineHCID 7679Phenylacetyl chlorideHCID 23338990HCID 23338990, 화합물

생성물 1

HCID 23339068HCID 23339068, 화합물

시약·촉매·용매 1

HCID 241Benzene용매2회

실험 절차

To a stirred solution of 8 parts of ethyl 4-[(2,6-dimethylphenyl)amino]-1-piperidinecarboxylate in 4 parts of pyridine and 80 parts of benzene are added dropwise 7.7 parts of benzeneacetyl chloride in 40 parts of benzene. After the addition is complete, the whole is heated to reflux and stirred at reflux temperature for 3h.45. The reaction mixture is cooled and filtered. The benzene-phase is washed with water and then with sodium hydrogen carbonate solution and with water. After evaporation, an oily residue is obtained, which solidifies on triturating in 1,1'-oxybisethane, to yield 5 parts of ethyl 4-[N-(2,6-dimethylphenyl)-N-(phenylacetyl)amino]-1-piperidinecarboxylate; mp. 106° C.

후처리

  1. additionAfter the addition
  2. temperaturethe whole is heated
  3. temperatureto reflux
  4. temperatureat reflux temperature for 3h.45
  5. temperatureThe reaction mixture is cooled
  6. filtrationfiltered
  7. washThe benzene-phase is washed with water
  8. customAfter evaporation
  9. customan oily residue is obtained
  10. customon triturating in 1,1'-oxybisethane

출처 및 근거

ORD 기록
ord-957f4cc3100f4fe3b632dfa5941fc43c
출처 데이터셋
uspto-grants-1980_09
특허 번호
US04225606

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