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

HRID 838911

반응식

HRID 838911 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매HCID 14797Potassium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8648d9d6303043b8ac2671864212b58b
출처 데이터셋
uspto-grants-1978_06
특허 번호
US04093644

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