Piperidine → HCID 12393826、化合物

HRID 972724ノート

反応式

HRID 972724 の反応式
Br[CH2:2][CH2:3][CH2:4][C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][CH:6]=1.[NH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1>C1(C)C=CC=CC=1>[CH2:7]1[C:8]2[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:5]([CH2:4][CH2:3][CH2:2][N:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)=[CH:6]1

参加物

4

反応物 2

HCID 8082PiperidineHCID 105378211H-Indene, 3-(3-bromopropyl)-

生成物 1

HCID 12393826HCID 12393826、化合物収率 89%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

3-(3'-Bromopropyl)indene (94.8 g, 0.4 M) and piperidine (76 g, 0.9 M) are dissolved in 400 ml toluene. The mixture is heated under reflux 2 hours. After cooling, a large amount of solid is removed by filtration and washed with ether. The combined filtrate and washes are concentrated in vacuo. The residue is dissolved in ether and filtered to remove a small amount of insoluble material. The ether is removed in vacuo and the product is distilled collecting a fraction of 87.3 g (89% yield) boiling 132°-153°/0.05 mm.

後処理

  1. temperatureThe mixture is heated
  2. temperatureunder reflux 2 hours
  3. temperatureAfter cooling
  4. customa large amount of solid is removed by filtration
  5. washwashed with ether
  6. concentrationThe combined filtrate and washes are concentrated in vacuo
  7. dissolutionThe residue is dissolved in ether
  8. filtrationfiltered
  9. customto remove a small amount of insoluble material
  10. customThe ether is removed in vacuo
  11. distillationthe product is distilled
  12. customcollecting a fraction of 87.3 g (89% yield)
  13. customboiling 132°-153°

出典と根拠

ORDレコード
ord-e142dc216dd74c558b52a079c0bec999
出典データセット
uspto-grants-1977_10
特許番号
US04053596

反応ノート

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