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

HRID 1266930
ノート
印刷プレビュー

反応式

HRID 1266930 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228Dimethylformamide2 回HCID 64092,2,2-TrifluoroethanolHCID 11430Potassium CarbonateHCID 612733,5-Dichloro-2,4,6-trifluoropyridine

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water
溶媒

反応条件

温度
30 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-739964c9f58f41cd846ebea9cf3e870e
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06551682B1

反応ノート

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