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Hydrochloric Acid → 5-(Aminomethyl)-2-chloropyridine

HRID 483349
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HRID 483349 반응식
O.NN.[Cl:4][C:5]1[N:10]=[CH:9][C:8]([CH2:11][N:12]2C(=O)C3=CC=CC=C3C2=O)=[CH:7][CH:6]=1.Cl>C(O)C>[Cl:4][C:5]1[N:10]=[CH:9][C:8]([CH2:11][NH2:12])=[CH:7][CH:6]=1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 143247132-[(6-Chloropyridin-3-yl)methyl]-1H-isoindole-1,3(2H)-dione

생성물 1

HCID 70209275-(Aminomethyl)-2-chloropyridine수율 91.2%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
20 °C

실험 절차

Hydrazine hydrate (2.00 ml, 0.04 mol) was added at ambient temperature (20° C.) to a solution of N-(6-chloro-3-pyridylmethyl) phthalimide (10.70 g, 0.039 mol) in ethanol (150 ml), and the resulting solution was heated under reflux for 4 hours before being cooled to ambient temperature (20° C.). 25% w/v aqueous hydrochloric acid (60 ml) was added directly and the resulting mixture was heated under reflux for 1 hour. The reaction mixture was then cooled to ambient temperature (20° C.), filtered and evaporated under reduced pressure. The resulting concentrated mixture was filtered and the filtrate was cooled, with ice/salt bath cooling, and solid potassium hydroxide was added with stirring until the mixture became basic. The reaction mixture was then extracted with diethylether (5×150 ml). The combined ether extracts were dried using magnesium sulphate and evaporated under reduced pressure to give the product, 6-chloro-3-pyridylmethylamine as a brown oil (5.07 g, 90.6%).

후처리

  1. temperaturethe resulting solution was heated
  2. temperatureunder reflux for 4 hours
  3. additionwas added directly
  4. temperaturethe resulting mixture was heated
  5. temperatureunder reflux for 1 hour
  6. temperatureThe reaction mixture was then cooled to ambient temperature (20° C.)
  7. filtrationfiltered
  8. customevaporated under reduced pressure
  9. concentrationThe resulting concentrated mixture
  10. filtrationwas filtered
  11. temperaturethe filtrate was cooled, with ice/salt bath
  12. temperaturecooling
  13. additionsolid potassium hydroxide was added
  14. extractionThe reaction mixture was then extracted with diethylether (5×150 ml)
  15. dry with materialThe combined ether extracts were dried
  16. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-4eb7fe6c50ea4ed0b0c6280373870af8
출처 데이터셋
uspto-grants-1993_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05225423

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