反应 #2171045
ord-6e9dccf8f1924bcca10f01ffe973992f
反应方程式
dimethylacetamide
phosphorus oxychloride
NaOH
2-benzylindole
→
titled compound
收率 53.0%
3-Acetyl-2-benzylindole
收率 53.0%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他prepared in accordance with the literature (Khim.Geterotsikl.Soedin.1994,p133))
- 2workup.STIRRINGAfter stirring for 2 hours at 100° C.
- 3萃取extracted with ethyl acetate
- 4洗涤The extract was washed with water
- 5其他dried
- 6浓缩concentrated
- 7洗涤The obtained crystal was washed with n-hexane
实验过程
To a solution of 29.5 g (39 mmol) of dimethylacetamide was added dropwise under ice-cooling 7.00 g (76.9 mmol) of phosphorus oxychloride. After stirring for 30 min at room temperature, to the mixture was added 8,00 g (38.6 mmol) of 2-benzylindole (prepared in accordance with the literature (Khim.Geterotsikl.Soedin.1994,p133)). After stirring for 2 hours at 100° C., the mixture was poured to ice-water, neutralized with 2N NaOH, extracted with ethyl acetate. The extract was washed with water, dried, and concentrated. The obtained crystal was washed with n-hexane to give 5.1 g of the titled compound. Yield: 52%.