N-methyl-2-pyrrolidone → 1-Fluoro-2-iodo-3-nitrobenzene
反応式
FC(F)(F)S(O[C:7]1[C:12]([N+:13]([O-:15])=[O:14])=[CH:11][CH:10]=[CH:9][C:8]=1[F:16])(=O)=O.[I-:19].[Li+].CN1CCCC1=O>O>[I:19][C:7]1[C:8]([F:16])=[CH:9][CH:10]=[CH:11][C:12]=1[N+:13]([O-:15])=[O:14]参加物
5
実験手順
A mixture consisting of 2-fluoro-6-nitrophenyl trifluoromethanesulfonate (62.0 g, 0.215 mol), lithium iodide (60 g, 0.451 mol) and 1-methyl-2-pyrrolidinone (400 mL) was heated with stirring at 130°-132° C. (oil bath temperature) for 18 hours. Upon cooling it was poured into water (1200 mL) and extracted with diethyl ether. The combined extracts were washed with 1N NaOH, water and with brine. The solution was dried (MgSO4), filtered, and concentrated in vacuo to give 27.0 g of the title compound as a brown-colored solid title compound (m.p. 54°-57° C.).
後処理
- temperaturewas heated
- temperatureUpon cooling it
- extractionextracted with diethyl ether
- washThe combined extracts were washed with 1N NaOH, water and with brine
- dry with materialThe solution was dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-113e88db99fa49daa56870e69776ce96
- 出典データセット
- uspto-grants-1989_04
- 特許番号
- US04822781
反応ノート
読み込み中…