Methyl iodide → Benzilic acid
反応式
F[C:2]1[CH:19]=[CH:18][C:5]([C:6]([C:11]2[CH:16]=[CH:15][C:14](F)=[CH:13][CH:12]=2)([OH:10])[C:7]([OH:9])=[O:8])=[CH:4][CH:3]=1.[O-]CC.[Na+].[Na].CI>C(O)C>[C:7]([OH:9])(=[O:8])[C:6]([C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)([C:5]1[CH:18]=[CH:19][CH:2]=[CH:3][CH:4]=1)[OH:10]参加物
6
実験手順
25.0 g (0.095 mol) of 4,4′-difluorobenzilic acid is added to freshly prepared sodium ethoxide solution containing 2.17 g (0.095 mol) of sodium and 200 ml of ethanol at 20° C. and stirred for 3 hours. The solution is evaporated to dryness, the residue is dissolved in DMF, 22.57 g (0.16 mol) of methyl iodide is added dropwise at 20° C., and the mixture is stirred for 24 hours. It is worked up and purified analogously to compound 12b. Yield: 21.06 g (80% of theory).
後処理
- customThe solution is evaporated to dryness
- dissolutionthe residue is dissolved in DMF
- stirringthe mixture is stirred for 24 hours
- custompurified analogously to compound 12b
出典と根拠
- ORDレコード
- ord-aef3a9165c004a55b2384744041b864a
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06852728B2
反応ノート
読み込み中…