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Toluene → Ethyl 4-[(4-chlorophenyl)imino]-1-piperidinecarboxylate

HRID 28127
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반응식

HRID 28127 반응식
O=[C:2]1[CH2:7][CH2:6][N:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:4][CH2:3]1.[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([NH2:20])=[CH:16][CH:15]=1.CC1C=CC=CC=1.CC1C=CC(S(O)(=O)=O)=CC=1>O>[Cl:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]=[C:2]2[CH2:7][CH2:6][N:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:4][CH2:3]2)=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1140TolueneHCID 6101p-Toluenesulfonic acidHCID 78124-ChloroanilineHCID 34767Ethyl 4-oxo-1-piperidinecarboxylate

생성물 1

HCID 14665236Ethyl 4-[(4-chlorophenyl)imino]-1-piperidinecarboxylate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 171.2 parts of ethyl 4-oxo-1-piperidinecarboxylate, 159.5 parts of 4-chlorobenzenamine, 1520 parts of anhydrous methylbenzene and a few crystals of 4-methylbenzenesulfonic acid is stirred and refluxed for 7 hours. (The reaction vessel is provided with a reflux-condensor and water-separator). The methylbenzene is evaporated and the oily residue is distilled in vacuo, yielding 192 parts of oily ethyl 4-[(4-chlorophenyl)imino]-1-piperidinecarboxylate; bp. 171°-176° C. at 0.4 mm. pressure.

후처리

  1. temperaturerefluxed for 7 hours
  2. custom(The reaction vessel is provided with
  3. temperaturea reflux-condensor
  4. customThe methylbenzene is evaporated
  5. distillationthe oily residue is distilled in vacuo

출처 및 근거

ORD 기록
ord-69afb760ce334456b0c8437bc4ff6a35
출처 데이터셋
uspto-grants-1980_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04225606

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