1,8-Diazabicyclo(5.4.0)undec-7-ene → 2,2,7-trifluoro-2H-benzo[b][1,4]oxazin-3(4H)-one
反応式
Br[C:2]([F:15])([F:14])[C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([F:12])=[CH:8][C:7]=1[OH:13])=[O:4].N12CCCN=C1CCCCC2>C1(C)C=CC=CC=1>[F:14][C:2]1([F:15])[O:13][C:7]2[CH:8]=[C:9]([F:12])[CH:10]=[CH:11][C:6]=2[NH:5][C:3]1=[O:4]参加物
4
反応条件
- 温度
- 80 °C
実験手順
To 2-bromo-2,2-difluoro-N-(4-fluoro-2-hydroxyphenyl)acetamide (33 g, 116 mmol) in dry Toluene was added 1,8-Diazabicyclo[5.4.0]undec-7-en (DBU, 17.51 ml, 116 mmol). The resulting mixture was stirred overnight at 80° C. The reaction was quenched in saturated aqueous NH4Cl solution and extracted with ethyl acetate. The combined extracts were washed with brine, dried with Na2SO4 and concentrated to afford 24.94 g of the title compound.
後処理
- customThe reaction was quenched in saturated aqueous NH4Cl solution
- extractionextracted with ethyl acetate
- washThe combined extracts were washed with brine
- dry with materialdried with Na2SO4
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-f03a0203f5c543ae8c2180ee3cf09dcb
- 出典データセット
- uspto-grants-2014_06
- 特許番号
- US08754008B2
反応ノート
読み込み中…