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Water → 2-Bromo-4-(3-(trifluoromethyl)phenyl)thiazole

HRID 2263297
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HRID 2263297 반응식
[BrH:1].C(O)(=O)C.O=[C:7]([C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=1)[CH2:8][S:9][C:10]#[N:11].O>C(O)(=O)C>[Br:1][C:10]1[S:9][CH:8]=[C:7]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=2)[N:11]=1
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참가 물질

5

반응물 3

HCID 962WaterHCID 21893785Acetic Acid Mixture with Hydrobromic AcidHCID 862452532-Oxo-2-[3-(trifluoromethyl)phenyl]ethyl thiocyanate

생성물 1

HCID 469119962-Bromo-4-(3-(trifluoromethyl)phenyl)thiazole수율 59.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
130 °C

실험 절차

A 25% hydrogen bromide/acetic acid (35 ml) solution was added to a solution of 2-oxo-2-[3-(trifluoromethyl)phenyl]ethyl thiocyanate (3.88 g, 15.8 mmol) in acetic acid (35 ml), and the mixture was stirred at 130° C. for 2 hours and at room temperature for 1 hour. 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 2.88 g (59.1%) 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-55fbb2e366f74911bf6a9c923abcefba
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07851473B2

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