Methyl iodide → Methyl 2-(1,3-dioxaindan-5-yl)acetate
反応式
[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH2:10][C:11]([OH:13])=[O:12])=[CH:4][C:3]=2[O:2]1.[C:14](=O)([O-])[O-].[Cs+].[Cs+].CI>CN(C=O)C>[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH2:10][C:11]([O:13][CH3:14])=[O:12])=[CH:4][C:3]=2[O:2]1参加物
5
実験手順
A mixture of (3,4-methylenedioxyphenyl)acetic acid (4.64 g, 25.74 mmol) in dry DMF (40 mL), cesium carbonate (9.2 g, 25.74 mmol) and methyl iodide (3.7 g, 26.0 mmol) in dry DMF (40 mL) was stirred at room temperature for 3h. At the end of this period, the reaction mixture was poured into ice water and extracted with ethyl acetate. The organic phase was washed with saturated NaHCO3, water, brine and then dried (MgSO4) and filtered. The filtrate was concentrated in vacuo to provide pure methyl (3,4-methylenedioxyphenyl)acetate as an oil (4.38 g).
後処理
- extractionextracted with ethyl acetate
- washThe organic phase was washed with saturated NaHCO3, water, brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo
出典と根拠
- ORDレコード
- ord-65362d73281c489fac77eb543a1e8af0
- 出典データセット
- uspto-grants-1995_02
- 特許番号
- US05391566
反応ノート
読み込み中…