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

HRID 1885720ノート

反応式

HRID 1885720 の反応式
[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

参加物

5

反応物 2

HCID 6115AnilineHCID 51700761-Benzyl-2-piperidone

生成物 1

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

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 1140Toluene溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-8b5809c6ad374b10a5bddd9673c4ab7d
出典データセット
uspto-grants-1992_09
特許番号
US05145967

反応ノート

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