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Bromopinacolone → 2-(4-Allyl-1-piperazinyl)-4-tert.butyl-thiazole

HRID 461780
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HRID 461780 반응식
[CH2:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([NH2:12])=[S:11])[CH2:6][CH2:5]1)[CH:2]=[CH2:3].[CH3:13][C:14]([C:17]([CH2:19]Br)=O)([CH3:16])[CH3:15]>C(O)C>[CH2:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]2[S:11][CH:19]=[C:17]([C:14]([CH3:16])([CH3:15])[CH3:13])[N:12]=2)[CH2:6][CH2:5]1)[CH:2]=[CH2:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21642BromopinacoloneHCID 47405064-prop-2-enylpiperazine-1-carbothioamide

생성물 1

HCID 213924772-(4-Allyl-1-piperazinyl)-4-tert.butyl-thiazole

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

3.7 g of 4-allyl-1-piperazinyl-thiocarboxamide are added to a solution of 3.6 g of bromopinacoline in 40 cc of ethanol, and the reaction mixture is subsequently heated to the boil at reflux for 2 hours. The mixture is subsequently concentrated by evaporation in a vacuum, the residue is dissolved in a small amount of water and divided between ether and a concentrated aqueous sodium hydroxide solution. The ether phase is washed with water, dried over sodium sulphate and saturated with hydrogen chloride gas after filtration. The monohydrochloride of 2-(4-allyl-1-piperazinyl)-4-tert.butyl-thiazole crystallizes and has an M.P. of 212°-214° after recrystallization from ethanol/diisopropyl ether.

후처리

  1. temperaturethe reaction mixture is subsequently heated to the boil
  2. temperatureat reflux for 2 hours
  3. concentrationThe mixture is subsequently concentrated by evaporation in a vacuum
  4. dissolutionthe residue is dissolved in a small amount of water
  5. washThe ether phase is washed with water
  6. dry with materialdried over sodium sulphate and saturated with hydrogen chloride gas
  7. filtrationafter filtration
  8. customThe monohydrochloride of 2-(4-allyl-1-piperazinyl)-4-tert.butyl-thiazole crystallizes
  9. customafter recrystallization from ethanol/diisopropyl ether

출처 및 근거

ORD 기록
ord-aeffb55f95fd41658204d7f3c3b97d7a
출처 데이터셋
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04064244

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