Water → Thiazole, 2-bromo-4-(3-methylphenyl)-

HRID 2263303노트

반응식

HRID 2263303 반응식
[BrH:1].C(O)(=O)C.[CH3:6][C:7]1[CH:8]=[C:9]([C:13](=O)[CH2:14][S:15][C:16]#[N:17])[CH:10]=[CH:11][CH:12]=1.O>C(O)(=O)C>[Br:1][C:16]1[S:15][CH:14]=[C:13]([C:9]2[CH:10]=[CH:11][CH:12]=[C:7]([CH3:6])[CH:8]=2)[N:17]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 21893785Acetic Acid Mixture with Hydrobromic AcidHCID 862450512-(3-Methylphenyl)-2-oxoethyl thiocyanate

생성물 1

HCID 49758214Thiazole, 2-bromo-4-(3-methylphenyl)-수율 66.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
130 °C

실험 절차

A 25% hydrogen bromide/acetic acid (20 ml) solution was added to a solution of 2-(3-methylphenyl)-2-oxoethyl thiocyanate (2.29 g, 12.0 mmol) in acetic acid (20 ml), and the mixture was stirred at 130° C. for 2 hours. Water was poured to the reaction mixture, and the mixture was extracted with chloroform. The extract was washed with water, and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1) to give 2.03 g (66.8%) of the desired product as an oil.

후처리

  1. extractionthe mixture was extracted with chloroform
  2. washThe extract was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=9:1)

출처 및 근거

ORD 기록
ord-406f9e775fb441d9957df316f39d8671
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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