Government regulation → 7-Bromo-5-chloro-2,3-dihydrobenzofuran
反应方程式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][CH2:8][CH2:7][C:6]=2[CH:10]=1.[Br:11]Br.S([O-])([O-])(=O)=S.[Na+].[Na+]>C(O)(=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([Br:11])[C:5]2[O:9][CH2:8][CH2:7][C:6]=2[CH:10]=1参与物
5
实验过程
To a stirred solution of (33) (1.84 g, 11.93 mmol) in acetic acid (10 ml) at 0° C., was slowly added a solution of bromine (1.24 ml, 24 mmol) in acetic acid (5 ml). The reaction mixture was stirred at room temperature for 4.5 h. A 10% sodium thiosulphate solution (70 ml) was added and the mixture stirred for 10 min. The bulk of the solvent was evaporated in vacuo. The resulting oil was dissolved in ether (50 ml), washed with water (20 ml), saturated NaHCO2 (2×15 ml), brine (1×15 ml), dried Na2SO4 and evaporated in vacuo to give 2.55 g (92%) of (34) as a oil.
后处理
- stirringthe mixture stirred for 10 min
- customThe bulk of the solvent was evaporated in vacuo
- dissolutionThe resulting oil was dissolved in ether (50 ml)
- washwashed with water (20 ml), saturated NaHCO2 (2×15 ml), brine (1×15 ml), dried Na2SO4
- customevaporated in vacuo
来源与证据
- ORD记录
- ord-f2c2ef8aac97430eba3688d429ad02ec
- 来源数据集
- uspto-grants-1993_11
- 专利号
- US05262430
反应笔记
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