Aniline → N-[1-(Phenylmethyl)-4-piperidinylidene]benzenamine

HRID 1885720노트

반응식

HRID 1885720 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][CH2:11][CH2:10][C:9]1=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>C1(C)C=CC(S(O)(=O)=O)=CC=1.C1(C)C=CC=CC=1>[CH2:1]([N:8]1[CH2:13][CH2:12][C:11](=[N:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[CH2:10][CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 2

HCID 6115AnilineHCID 51700761-Benzyl-2-piperidone

생성물 1

HCID 13860895N-[1-(Phenylmethyl)-4-piperidinylidene]benzenamine수율 65%

시약·촉매·용매 2

HCID 6101p-Toluenesulfonic acid촉매HCID 1140Toluene용매

실험 절차

A 1000 ml round bottom flask affixed with a stirring bar, a Dean-Stark trap and a condenser was charged with 101.6 g of benzylpiperidone, 500 ml of toluene, 50 g of aniline and 500 mg of p-toluene sulfonic acid. The mixture was refluxed overnight. After removal of the solvent, the reaction mixture was poured into 600 ml of isopropyl ether. The resulting solution was filtered, and the filtrate concentrated and then vacuum distilled at 185°-190° C., 1.25 torr to obtain 91.9 g (about 65% yield) of product as a light yellow oil.

후처리

  1. customA 1000 ml round bottom flask affixed with a stirring bar
  2. temperatureThe mixture was refluxed overnight
  3. customAfter removal of the solvent
  4. additionthe reaction mixture was poured into 600 ml of isopropyl ether
  5. filtrationThe resulting solution was filtered
  6. concentrationthe filtrate concentrated
  7. distillationvacuum distilled at 185°-190° C.

출처 및 근거

ORD 기록
ord-8b5809c6ad374b10a5bddd9673c4ab7d
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05145967

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