Potassium Fluoride → 2,4-Dinitro-5-fluorophenoxyacetonitrile

HRID 1381634ノート

反応式

HRID 1381634 の反応式
[N+:1]([C:4]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[C:11](Cl)=[CH:10][C:5]=1[O:6][CH2:7][C:8]#[N:9])([O-:3])=[O:2].[F-:18].[K+]>CS(C)=O>[N+:1]([C:4]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[C:11]([F:18])=[CH:10][C:5]=1[O:6][CH2:7][C:8]#[N:9])([O-:3])=[O:2]

参加物

4

反応物 2

HCID 522689Potassium FluorideHCID 14250577(5-Chloro-2,4-dinitrophenoxy)acetonitrile

生成物 1

HCID 140535322,4-Dinitro-5-fluorophenoxyacetonitrile収率 89.3%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A suspension of 2,4-dinitro-5-chlorophenoxyacetonitrile (5.0 g) and potassium fluoride (1.7 g) in dimethylsulfoxide (25 g) was stirred at 83° to 85° C. for 1 hour. The reaction mixture was poured into ice-water (300 ml) and extracted with ethyl acetate. The organic layer was washed with water, dried over magnesium sulfate and concentrated. The precipitated crystals were collected by filtration and washed with ether to give crystalline 2,4-dinitro-5-fluorophenoxyacetonitrile (4.18 g; yield, 89.3%). M.P., 118°-118.5° C. (recrystallized from methanol).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. filtrationThe precipitated crystals were collected by filtration
  6. washwashed with ether

出典と根拠

ORDレコード
ord-9e9df53f52724bdda0be8e41cc5f438a
出典データセット
uspto-grants-1989_02
特許番号
US04803270

反応ノート

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