Chlorodifluoromethane → 1-[1-(Difluoromethoxy)naphthalen-2-yl]ethan-1-one

HRID 129467

反応式

HRID 129467 の反応式
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[C:12](=[O:14])[CH3:13].[OH-].[Na+].[F:17][CH:18]([F:20])Cl>O1CCOCC1>[F:17][CH:18]([F:20])[O:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[C:12](=[O:14])[CH3:13]

参加物

5

反応物 3

HCID 6372ChlorodifluoromethaneHCID 14798Sodium HydroxideHCID 697331'-Hydroxy-2'-acetonaphthone

生成物 1

HCID 23608281-[1-(Difluoromethoxy)naphthalen-2-yl]ethan-1-one

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

10 g of 1-hydroxy-2-acetylnaphthalene are dissolved in 60 ml of dioxane, and 30 ml of 30% sodium hydroxide solution are added. At a temperature of from 70° C. to 80° C., difluorochloromethane (Freon 22) is introduced until no further absorption is observed. The dioxane phase is then decanted, the NaOH phase is washed with dioxane, the dioxane phase is decanted, and the combined dioxane solutions are largely concentrated in vacuo using a rotary evaporator. Water is added to the residue, the mixture is extracted several times with diethyl ether, and the diethyl ether solution is dried over Na2SO4, filtered and concentrated by evaporation. The residue is recrystallised from diethyl ether/hexane. Yield: 4 g, m.p. 80°-81° C.

後処理

  1. customThe dioxane phase is then decanted
  2. washthe NaOH phase is washed with dioxane
  3. customthe dioxane phase is decanted
  4. concentrationthe combined dioxane solutions are largely concentrated in vacuo
  5. customa rotary evaporator
  6. additionWater is added to the residue
  7. extractionthe mixture is extracted several times with diethyl ether
  8. dry with materialthe diethyl ether solution is dried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated by evaporation
  11. customThe residue is recrystallised from diethyl ether/hexane

出典と根拠

ORDレコード
ord-2b18abdb79884dd28e51164fd3827cd8
出典データセット
uspto-grants-1995_11
特許番号
US05468751

関連ノート

読み込み中…