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

HRID 65454

反応式

HRID 65454 の反応式
[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]

参加物

7

反応物 3

HCID 113352,6-DimethylphenolHCID 522689Potassium FluorideHCID 608182Tetrafluoroisophthalonitrile

生成物 1

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

試薬・触媒・溶媒 3

HCID 180Acetone溶媒HCID 6342Acetonitrile溶媒HCID 8078Cyclohexane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-9472bc0a7bf046da91c69ec8bf50cbce
出典データセット
uspto-grants-1986_09
特許番号
US04614742

関連ノート

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