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

HRID 1840713

반응식

HRID 1840713 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

반응 조건

온도
10 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d32f779d34df45009dd0456ed55a88ee
출처 데이터셋
uspto-grants-2004_01
특허 번호
US06683029B1

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