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Dimethylformamide → 3,5-Dichloro-2-fluoro-4,6-bis(2,2,2-trifluoroethoxy)pyridine

HRID 1266930
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HRID 1266930 반응식
[Cl:1][C:2]1[C:3](F)=[N:4][C:5]([F:10])=[C:6]([Cl:9])[C:7]=1F.CN([CH:15]=[O:16])C.C(=O)([O-])[O-].[K+].[K+].[F:23][C:24]([F:28])([F:27])[CH2:25][OH:26]>O>[Cl:9][C:6]1[C:5]([F:10])=[N:4][C:3]([O:16][CH2:15][C:24]([F:28])([F:27])[F:23])=[C:2]([Cl:1])[C:7]=1[O:26][CH2:25][C:24]([F:28])([F:27])[F:23]
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참가 물질

6

반응물 4

HCID 6228Dimethylformamide2회HCID 64092,2,2-TrifluoroethanolHCID 11430Potassium CarbonateHCID 612733,5-Dichloro-2,4,6-trifluoropyridine

생성물 1

HCID 185448013,5-Dichloro-2-fluoro-4,6-bis(2,2,2-trifluoroethoxy)pyridine

시약·촉매·용매 1

HCID 962Water
용매

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온도
30 °C

실험 절차

A reaction flask was loaded with 3,5-dichloro-2,4,6-trifluoropyridine (5.6 g), DMF (15 ml), and potassium carbonate (9.2 g), and heated up to 30° C. with stirring. To this, a mixture of 2,2,2-trifluoroethanol (5.6 g) and DMF (10 ml) was dropwise added in one hour. After the dropwise addition was ended, the temperature was raised to 50° C., followed by stirring for three hours. The heating was stopped and left to cool. Thereafter, water (100 ml) was added to the reaction mixture, followed by extraction with ether. The ether layer was condensed to give 3,5-dichloro-2-fluoro-4,6-bis(2,2,2-trifluoroethoxy)pyridine (9.7 g). By GC/MS analysis, a molecular ion peak of 362 was confirmed.

후처리

  1. additionwas dropwise added in one hour
  2. additionAfter the dropwise addition
  3. temperaturethe temperature was raised to 50° C.
  4. stirringby stirring for three hours
  5. waitleft
  6. temperatureto cool
  7. extractionfollowed by extraction with ether
  8. customcondensed

출처 및 근거

ORD 기록
ord-739964c9f58f41cd846ebea9cf3e870e
출처 데이터셋
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06551682B1

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