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2-Bromo-1-(4-hydroxyphenyl)ethanone → HCID 67337013, 화합물

HRID 910648
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HRID 910648 반응식
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1)=O.[Br:12][C:13]1[C:14]([NH2:19])=[N:15][CH:16]=[CH:17][CH:18]=1>C(#N)C>[Br:12][C:13]1[C:14]2[N:15]([CH:2]=[C:3]([C:5]3[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=3)[N:19]=2)[CH:16]=[CH:17][CH:18]=1
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참가 물질

4

반응물 2

HCID 49642-Bromo-1-(4-hydroxyphenyl)ethanoneHCID 8177002-Amino-3-bromopyridine

생성물 1

HCID 67337013HCID 67337013, 화합물수율 63.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
110 °C

실험 절차

432 mg (corresponding to 2.01 mmol) of 2-bromo-4′-hydroxyacetophenone and 348 mg (corresponding to 2.01 mmol) of 3-bromo-2-aminopyridine were dissolved in 20 mL of acetonitrile. The resulting solution was refluxed in an oil bath at 110° C. for 6 hours. After the completion of the reaction, the reaction solution was cooled down to room temperature, and precipitates were filtered and recovered. The precipitates were washed with acetonitrile and dried under reduced pressure. The resulting crude crystals were suspended in a mixed solution of 8 mL of water and 8 mL of methanol. Then, about 8 mL of a saturated sodium hydrogencarbonate solution was added thereto, and the mixture was sonicated for 5 minutes using an ultrasonic washing machine. Precipitates were filtered and recovered from the resulting mixture, sufficiently washed with water, and dried under reduced pressure, to obtain 368 mg (corresponding to 1.27 mmol) of 8-bromo-2-(4′-hydroxyphenyl)imidazo[1,2-a]pyridine (FIG. 13, Step 2).

후처리

  1. customAfter the completion of the reaction
  2. temperaturethe reaction solution was cooled down to room temperature
  3. customprecipitates
  4. filtrationwere filtered
  5. customrecovered
  6. washThe precipitates were washed with acetonitrile
  7. customdried under reduced pressure
  8. additionThen, about 8 mL of a saturated sodium hydrogencarbonate solution was added
  9. customthe mixture was sonicated for 5 minutes
  10. customPrecipitates
  11. filtrationwere filtered
  12. customrecovered from the resulting mixture
  13. washsufficiently washed with water
  14. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-76138d6a59c44d89935e93bd8d51e52b
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022207B2

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