1,1-Dichloro-2,2-difluoroethene → 2-(2,2-Dichloro-1,1-difluoroethoxy)-4-methyl-1-nitrobenzene

HRID 838911ノート

反応式

HRID 838911 の反応式
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([N+:9]([O-:11])=[O:10])=[C:6]([OH:8])[CH:7]=1.[Cl:12][C:13]([Cl:17])=[C:14]([F:16])[F:15]>CC(C)=O.[OH-].[K+]>[Cl:12][CH:13]([Cl:17])[C:14]([F:16])([F:15])[O:8][C:6]1[CH:7]=[C:2]([CH3:1])[CH:3]=[CH:4][C:5]=1[N+:9]([O-:11])=[O:10]

参加物

5

反応物 2

HCID 65921,1-Dichloro-2,2-difluoroetheneHCID 127886-Nitro-m-cresol

生成物 1

HCID 203252622-(2,2-Dichloro-1,1-difluoroethoxy)-4-methyl-1-nitrobenzene収率 27%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 14797Potassium Hydroxide溶媒

実験手順

In a 500 ml stirred reaction flask equipped with thermometer, air condenser, dropping funnel and ice water bath was placed 76.57 g (0.5 mol) of 5-methyl-2-nitrophenol in 150 ml of acetone and 5.5 g of powdered KOH (85 percent). The mixture was vigorously stirred at 10° C, whereupon 73 g of 2,2-dichloro-1,1-difluoroethene was gradually introduced. After stirring overnight, the reaction mixture was poured into ice water, and the lower organic layer separated by methylene chloride extraction. The extract was washed with diluted bicarbonate of soda solution, decolorized with charcoal, and dried over desiccant-grade magnesium sulfate. Evaporation of the solvent left an oily residue which was vacuum distilled at 5 mm to give 38.6 g of 2-(2,2-dichloro-1,1-difluoroethoxy)-4-methyl-1-nitrobenzene distilling at 156° C.

後処理

  1. customreaction flask
  2. customequipped with thermometer, air condenser
  3. additionwas gradually introduced
  4. stirringAfter stirring overnight
  5. customthe lower organic layer separated by methylene chloride extraction
  6. washThe extract was washed with diluted bicarbonate of soda solution
  7. dry with materialdried over desiccant-grade magnesium sulfate
  8. customEvaporation of the solvent
  9. waitleft an oily residue which
  10. distillationdistilled at 5 mm

出典と根拠

ORDレコード
ord-8648d9d6303043b8ac2671864212b58b
出典データセット
uspto-grants-1978_06
特許番号
US04093644

反応ノート

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