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2-Methoxyethanol → HCID 21388644, 화합물

HRID 1833291
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HRID 1833291 반응식
[OH-].[K+].[NH2:3][C:4]1[C:9]([Cl:10])=[CH:8][N:7]=[C:6](Cl)[C:5]=1[Cl:12].[CH3:13][O:14][CH2:15][CH2:16][OH:17]>>[NH2:3][C:4]1[C:9]([Cl:10])=[CH:8][N:7]=[C:6]([O:17][CH2:16][CH2:15][O:14][CH3:13])[C:5]=1[Cl:12]
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참가 물질

4

반응물 3

HCID 80192-Methoxyethanol2회HCID 14797Potassium HydroxideHCID 7286762,3,5-trichloropyridin-4-amine

생성물 1

HCID 21388644HCID 21388644, 화합물

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온도
118 °C

실험 절차

A solution of 16.5 grams (0.25 mole) of 86 percent potassium hydroxide dissolved in 100 milliliters of 2-methoxyethanol was added to a mixture of 49.5 grams (0.25 mole) of 4-amino-2,3,5-trichloropyridine in 150 milliliters of 2-methoxyethanol. The mixture was heated, with agitation, to 118° C. and held between 118°-120° C. for 31/2 hours. The reaction mixture was cooled to 75° C. and filtered under reduced pressure to remove the insoluble solids. The excess 2-methoxyethanol was evaporated off under reduced pressure and the liquid residue remaining was crystallized from hexane. The 4-amino-3,5-dichloro-2-(2-methoxyethoxy)pyridine product was recovered by filtration under reduced pressure, and obtained in a yield of 57 grams melting at 92°-93.5° C.

후처리

  1. customheld between 118°-120° C. for 31
  2. custom2 hours
  3. temperatureThe reaction mixture was cooled to 75° C.
  4. filtrationfiltered under reduced pressure
  5. customto remove the insoluble solids
  6. customThe excess 2-methoxyethanol was evaporated off under reduced pressure
  7. customthe liquid residue remaining was crystallized from hexane
  8. filtrationThe 4-amino-3,5-dichloro-2-(2-methoxyethoxy)pyridine product was recovered by filtration under reduced pressure
  9. customobtained in a yield of 57 grams melting at 92°-93.5° C.

출처 및 근거

ORD 기록
ord-d2f980471b104de089d8c252199c917c
출처 데이터셋
uspto-grants-1978_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04066438

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