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

HRID 1733266
ノート
印刷プレビュー

反応式

HRID 1733266 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d4413a4440cb404099fed1e0568d214c
出典データセット
uspto-grants-1980_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04241058

反応ノート

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