六氢吡啶 → HCID 12393826，化合物

HRID 972724笔记

反应方程式

HRID 972724 反应方程式
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

参与物

4

反应物 2

HCID 8082六氢吡啶HCID 105378211H-Indene, 3-(3-bromopropyl)-

产物 1

HCID 12393826HCID 12393826，化合物收率 89%

试剂、催化剂与溶剂 1

HCID 1140甲苯溶剂

实验过程

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.

后处理

  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°

来源与证据

ORD记录
ord-e142dc216dd74c558b52a079c0bec999
来源数据集
uspto-grants-1977_10
专利号
US04053596

反应笔记

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