Piperidine → HCID 12393826, 화합물

HRID 972724노트

반응식

HRID 972724 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 12393826HCID 12393826, 화합물수율 89%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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°

출처 및 근거

ORD 기록
ord-e142dc216dd74c558b52a079c0bec999
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04053596

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