2,4-Dinitrophenol → 2,4-Dinitroanisole

HRID 621828

反応式

HRID 621828 の反応式
[N+:1]([C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:5]=1[OH:13])([O-:3])=[O:2].[C:14](=O)([O-])[O-].[K+].[K+].CBr>C(C(C)=O)C(C)C>[N+:1]([C:4]1[CH:9]=[C:8]([N+:10]([O-:12])=[O:11])[CH:7]=[CH:6][C:5]=1[O:13][CH3:14])([O-:3])=[O:2]

参加物

5

反応物 3

HCID 14932,4-DinitrophenolHCID 6323Methyl BromideHCID 11430Potassium Carbonate

生成物 1

HCID 83852,4-Dinitroanisole

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

A 1 liter reactor is charged with 300 ml of methyl isobutyl ketone, 79.17 g of 2,4-dinitrophenol (100%) and 175.9 g of ground potassium carbonate and 63.6 g of methyl bromide. The autoclave is closed and heated for 3 hours to 115°-120° C. (pressure: 3.5 bar). The temperature is then kept for a further 5 hours at 140°-142° C. (pressure: 5-3 bar, falling). After cooling to c. 25° C., the solvent is distilled off at 50° C. under a partial vacuum and the salt-containing residue is taken up in warm water. 2,4-Dinitroanisole is isolated by filtration and washed with 1% ammonia solution and with warm water of c. 50° C. and dried at 50° C. under vacuum, to give 84.6 g (91.2% yield) of 2,4-dinitroanisole with a titre of 91.8%.

後処理

  1. customThe autoclave is closed
  2. temperatureheated for 3 hours to 115°-120° C. (pressure: 3.5 bar)
  3. temperatureAfter cooling to c
  4. distillation25° C., the solvent is distilled off at 50° C. under a partial vacuum

出典と根拠

ORDレコード
ord-47e1fa568fa64076a96ab28e280ea2f0
出典データセット
uspto-grants-1989_04
特許番号
US04825005

関連ノート

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