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

HRID 544665
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HRID 544665 반응식
[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]
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참가 물질

4

반응물 2

HCID 7841Allyl bromideHCID 132096564,5-Bis-(p-methoxyphenyl)-thiazoline-2-thione

생성물 1

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

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5828c1b0d9d44180b13f046d1f8053a1
출처 데이터셋
uspto-grants-1984_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04451471

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