Water → 5,6-Difluoro-(3-fluorophenoxy)-pyrimidine

HRID 1840713

反応式

HRID 1840713 の反応式
[F:1][C:2]1[C:3]([F:9])=[N:4][C:5](F)=[N:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[F:16][C:17]1[CH:18]=[C:19]([OH:23])[CH:20]=[CH:21][CH:22]=1.O>C(#N)C>[F:1][C:2]1[CH:7]=[N:6][C:5]([O:23][C:19]2[CH:20]=[CH:21][CH:22]=[C:17]([F:16])[CH:18]=2)=[N:4][C:3]=1[F:9]

参加物

6

反応物 4

HCID 962WaterHCID 97433-FluorophenolHCID 11430Potassium CarbonateHCID 127973072,4,5-Trifluoropyrimidine

生成物 1

HCID 234439225,6-Difluoro-(3-fluorophenoxy)-pyrimidine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒2 回

反応条件

温度
10 °C

実験手順

11.38 g (0.085 mol) of trifluoropyrimidine are dissolved in 240 ml of acetonitrile and admixed with 15.26 g (0.11 mol) of potassium carbonate, and the mixture is cooled to 10° C. Under argon, a solution of 9.52 g (0.085 mol) of 3-fluorophenol in 80 ml of acetonitrile is added dropwise. The mixture is then stirred under argon, without further cooling, for another 18 hours. The mixture is poured into 1 litre of water and extracted three times with in each case 150 ml of ethyl acetate, and the organic phase is dried over sodium sulphate and concentrated under reduced pressure. The residue is subjected to kugelrohr distillation. This gives 15.2 g (79.1% of theory) of 5,6-difluoro-(3-fluorophenoxy)-pyrimidine of boiling point 95° C. at 0.5 mbar.

後処理

  1. extractionextracted three times with in each case 150 ml of ethyl acetate
  2. dry with materialthe organic phase is dried over sodium sulphate
  3. concentrationconcentrated under reduced pressure
  4. distillationdistillation

出典と根拠

ORDレコード
ord-d32f779d34df45009dd0456ed55a88ee
出典データセット
uspto-grants-2004_01
特許番号
US06683029B1

関連ノート

読み込み中…