反応式
[S:1]([OH:11])(=[O:10])([C:3]1[CH:8]=[CH:7][C:6]([NH2:9])=[CH:5][CH:4]=1)=[O:2].[N:12]([O-])=O.[Na+].[F:16][C:17]1[CH:22]=[CH:21][CH:20]=[C:19]([F:23])[C:18]=1[OH:24].[OH-].[K+]>O.Cl.O1CCOCC1>[F:16][C:17]1[CH:22]=[C:21]([N:12]=[N:9][C:6]2[CH:5]=[CH:4][C:3]([S:1]([OH:11])(=[O:10])=[O:2])=[CH:8][CH:7]=2)[CH:20]=[C:19]([F:23])[C:18]=1[OH:24]参加物
実験手順
Sulfanilic acid (0.767 g, 4.43 mmol) was dissolved in hot mixture of 20 mL of water and 10 mL of conc. HCl. The solution was cooled in ice/NaCl bath to 0° C. giving a suspension of HCl salt. The solution of sodium nitrite (0.367 g, 5.32 mmol in 5 mL of water) was added dropwise to the suspension of ammonium salt, maintaining the temperature below +5° C. All solid dissolved and the resulting solution was stirred for 20 min. After that white precipitate formed again and the resulting suspension was added dropwise to the mixture of 2,6-difluorophenol (0.576 g, 4.43 mmol) in 10 mL of dioxane and KOH (10 g) in 15 mL of water, cooled in ice/water bath. The reaction mixture was stirred for 30 min in ice/water bath and then extracted with ethyl acetate (3×30 mL). The aqueous solution was acidified with 10% HCl to pH 2-3 and the formed yellow precipitate was collected, washed with water and dried in vacuum to give phenol 2 as a yellow powder (1.1 g, 79%).
後処理
- customgiving
- temperaturemaintaining the temperature below +5° C
- dissolutionAll solid dissolved
- customAfter that white precipitate formed again
- extractionextracted with ethyl acetate (3×30 mL)
- customthe formed yellow precipitate was collected
- washwashed with water
- customdried in vacuum
出典と根拠
- ORDレコード
- ord-dea014818bc0461e92a40d7d87eca443
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09140706B2
関連ノート
読み込み中…