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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2-Pyridinamine, 5-iodo- → HCID 77985000, 화합물

HRID 1502652
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HRID 1502652 반응식
Br[CH2:2][C:3]([C:5]1[CH:6]=[CH:7][C:8]([N:11]2[CH:15]=[CH:14][CH:13]=[N:12]2)=[N:9][CH:10]=1)=O.[NH2:16][C:17]1[CH:22]=[CH:21][C:20]([I:23])=[CH:19][N:18]=1>C(#N)C>[N:11]1([C:8]2[CH:7]=[CH:6][C:5]([C:3]3[N:16]=[C:17]4[CH:22]=[CH:21][C:20]([I:23])=[CH:19][N:18]4[CH:2]=3)=[CH:10][N:9]=2)[CH:15]=[CH:14][CH:13]=[N:12]1
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참가 물질

4

반응물 2

HCID 885792-Pyridinamine, 5-iodo-HCID 86717669HCID 86717669, 화합물

생성물 1

HCID 77985000HCID 77985000, 화합물수율 55.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
100 °C

실험 절차

100.0 mg (corresponding to 0.38 mmol) of 5-(2-bromoacetyl)-2-(pyrazole-1-yl)pyridine and 83.6 mg (corresponding to 0.38 mmol) of 2-amino-5-iodopyridine were dissolved in 3.8 mL of acetonitrile. The resulting solution was heated under reflux for 4 hours in an oil bath at 100° C. After the completion of the reaction, the reaction solution was cooled down to room temperature, and precipitates were filtered. The precipitates were washed with acetonitrile and dried under reduced pressure. The resulting crude crystals were suspended in a mixed solution of 50 mL of water and 50 mL of methanol. Then, about 50 mL of a saturated sodium hydrogencarbonate solution was added thereto, and the mixture was sonicated for an hour using an ultrasonic washing machine. Precipitates were filtered from the resulting mixture, sufficiently washed with water, and dried under reduced pressure, to obtain 80.2 mg (corresponding to 0.21 mmol) of 2-[2-(pyrazole-1-yl)pyridine-5-yl]-6-iodoimidazo[1,2-a]pyridine (FIG. 5, step 3).

후처리

  1. temperatureThe resulting solution was heated
  2. customAfter the completion of the reaction
  3. temperaturethe reaction solution was cooled down to room temperature
  4. customprecipitates
  5. filtrationwere filtered
  6. washThe precipitates were washed with acetonitrile
  7. customdried under reduced pressure
  8. additionThen, about 50 mL of a saturated sodium hydrogencarbonate solution was added
  9. customthe mixture was sonicated for an hour
  10. customPrecipitates
  11. filtrationwere filtered from the resulting mixture
  12. washsufficiently washed with water
  13. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-00551d4550eb485ca089bda385f0aafb
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09211350B2

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