Pyridine → HCID 23339068、化合物

HRID 236746ノート

反応式

HRID 236746 の反応式
[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

参加物

5

反応物 3

HCID 1049PyridineHCID 7679Phenylacetyl chlorideHCID 23338990HCID 23338990、化合物

生成物 1

HCID 23339068HCID 23339068、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

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 3 h. 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.

後処理

  1. additionAfter the addition
  2. temperaturethe whole is heated
  3. temperatureto reflux
  4. temperatureat reflux temperature for 3 h
  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

出典と根拠

ORDレコード
ord-aad812be814f49f1bb82ce2c34cc9fcf
出典データセット
uspto-grants-1979_06
特許番号
US04157393

反応ノート

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