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Allyl bromide → 2-Allylthio-4,5-bis-(p-methoxyphenyl)-thiazole

HRID 544665
ノート
印刷プレビュー

反応式

HRID 544665 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:13]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)[S:12][C:11](=[S:22])[N:10]=2)=[CH:5][CH:4]=1.[CH2:23](Br)[CH:24]=[CH2:25]>[OH-].[Na+]>[CH2:25]([S:22][C:11]1[S:12][C:13]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)=[C:9]([C:6]2[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)[N:10]=1)[CH:24]=[CH2:23]
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 7841Allyl bromideHCID 132096564,5-Bis-(p-methoxyphenyl)-thiazoline-2-thione

生成物 1

HCID 132096752-Allylthio-4,5-bis-(p-methoxyphenyl)-thiazole

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

0.5 g of 4,5-bis-(p-methoxyphenyl)-thiazoline-2-thione are dissolved in 2.6 ml of 2 N sodium hydroxide solution while stirring. 0.367 g of allyl bromide is added, the mixture is stirred at room temperature for 10 minutes, extracted by shaking twice with 10 ml of toluene each time, the combined aqueous phases are washed twice with 5 ml of 2 N sodium hydroxide solution each time, dried over magnesium sulphate, concentrated by evaporation under reduced pressure and crystallised from hexane. 2-Allylthio-4,5-bis-(p-methoxyphenyl)-thiazole having a melting point of 57°-58° is obtained.

後処理

  1. stirringthe mixture is stirred at room temperature for 10 minutes
  2. extractionextracted
  3. stirringby shaking twice with 10 ml of toluene each time
  4. washthe combined aqueous phases are washed twice with 5 ml of 2 N sodium hydroxide solution each time
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated by evaporation under reduced pressure
  7. customcrystallised from hexane

出典と根拠

ORDレコード
ord-5828c1b0d9d44180b13f046d1f8053a1
出典データセット
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04451471

反応ノート

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