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

HRID 461780
ノート
印刷プレビュー

反応式

HRID 461780 の反応式
[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]
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 21642BromopinacoloneHCID 47405064-prop-2-enylpiperazine-1-carbothioamide

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-aeffb55f95fd41658204d7f3c3b97d7a
出典データセット
uspto-grants-1977_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04064244

反応ノート

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