2,6-Dimethylphenol → 2,4,5-Trifluoro-6-(2,6-xylyloxy)isophthalonitrile

HRID 65454

반응식

HRID 65454 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([CH3:8])[C:3]=1[OH:9].F[C:11]1[C:16]([C:17]#[N:18])=[C:15]([F:19])[C:14]([C:20]#[N:21])=[C:13]([F:22])[C:12]=1[F:23].[F-].[K+]>C(#N)C.CC(C)=O.C1CCCCC1>[F:19][C:15]1[C:14]([C:20]#[N:21])=[C:13]([F:22])[C:12]([F:23])=[C:11]([O:9][C:3]2[C:4]([CH3:8])=[CH:5][CH:6]=[CH:7][C:2]=2[CH3:1])[C:16]=1[C:17]#[N:18]

참가 물질

7

반응물 3

HCID 113352,6-DimethylphenolHCID 522689Potassium FluorideHCID 608182Tetrafluoroisophthalonitrile

생성물 1

HCID 136561882,4,5-Trifluoro-6-(2,6-xylyloxy)isophthalonitrile수율 77%

시약·촉매·용매 3

HCID 180Acetone용매HCID 6342Acetonitrile용매HCID 8078Cyclohexane용매

실험 절차

A solution of 1.2 g (10×10-3 mol) of 2,6-dimethylphenol in 40 ml of acetonitrile was dropwise added at a temperature of -10° C. to a solution of 2.0 g (10×10-3 mol) of tetrafluoroisophthalonitrile and 2.9 g (50×10-3 mol) of potassium fluoride. The mixture was allowed to stand at a temperature of -10° C. to 0° C. for 1 hour while stirring and the undissolved potassium fluoride was separated by filtration. The filtrate was concentrated to dryness in vacuo. The resultant residue was dissolved in a mixed solvent of acetone and cyclohexane and 2.3 g (77% yield) of the desired compound No. 37 was obtained as white crystal.

후처리

  1. customthe undissolved potassium fluoride was separated by filtration
  2. concentrationThe filtrate was concentrated to dryness in vacuo

출처 및 근거

ORD 기록
ord-9472bc0a7bf046da91c69ec8bf50cbce
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04614742

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