Water → 2-Bromo-4-(2-fluorophenyl)thiazole

HRID 2263176노트

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HRID 2263176 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=O)[CH2:9][S:10][C:11]#[N:12].[BrH:14].C(O)(=O)C.O>C(O)(=O)C>[Br:14][C:11]1[S:10][CH:9]=[C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[F:1])[N:12]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 18526224Thiocyanic acid, 2-(2-fluorophenyl)-2-oxoethyl esterHCID 21893785Acetic Acid Mixture with Hydrobromic Acid

생성물 1

HCID 687812882-Bromo-4-(2-fluorophenyl)thiazole수율 61.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
130 °C

실험 절차

To a solution of 2-(2-fluorophenyl)-2-oxoethyl thiocyanate (4.20 g, 21.5 mmol) in acetic acid (40 ml) was added a solution of 25% hydrogen bromide/acetic acid (40 ml), and the mixture was stirred at 130° C. for 2 hours. Water was poured into the reaction solution, 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 the desired product (3.41 g, 61.4%) 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-0dddba3fa67048e6a6b071751bd8556f
출처 데이터셋
uspto-grants-2010_12
특허 번호
US07851473B2

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