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Piperidine → 1-[3-(p-Tert.butyl-phenyl)-2-methyl-2-propenyl]-piperidine

HRID 1733266
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HRID 1733266 반응식
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([CH:11]=[C:12]([CH3:15])[CH2:13]Br)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[NH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1>CCOCC>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([CH:11]=[C:12]([CH3:15])[CH2:13][N:16]2[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2]
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참가 물질

4

반응물 2

HCID 8082PiperidineHCID 572041753-(p-Tert.butyl-phenyl)-2-methyl-allyl bromide

생성물 1

HCID 571057691-[3-(p-Tert.butyl-phenyl)-2-methyl-2-propenyl]-piperidine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

35 g of 3-(p-tert.butyl-phenyl)-2-methyl-allyl bromide in 70 ml of ether are added dropwise to a solution of 24.5 g of piperidine in 100 ml of absolute ether and the mixture is heated at reflux for 16 hours. The piperidine hydrobromide is removed by filtration and rinsed with ether. The ether solution is extracted with 2-N hydrochloric acid and made alkaline with 50% sodium hydroxide. The alkaline-aqueous solution is again extracted with ether, washed with water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 1-[3-(p-tert.butyl-phenyl)-2-methyl-2-propenyl]-piperidine of boiling point 96°-98° C./0.03 Torr.

후처리

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 16 hours
  3. customThe piperidine hydrobromide is removed by filtration
  4. washrinsed with ether
  5. extractionThe ether solution is extracted with 2-N hydrochloric acid
  6. extractionThe alkaline-aqueous solution is again extracted with ether
  7. washwashed with water
  8. dry with materialdried over sodium sulphate
  9. customevaporated
  10. distillationBy distillation there

출처 및 근거

ORD 기록
ord-d4413a4440cb404099fed1e0568d214c
출처 데이터셋
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04241058

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