反应 #2358149

ord-020b2000eff346e6b6f3553d6363f9ec

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他prepared in accordance with the literature (Khim.Geterotsikl.Soedin.1994,p133))
  2. 2
    workup.STIRRINGAfter stirring for 2 hours at 100° C.
  3. 3
    萃取extracted with ethyl acetate
  4. 4
    洗涤The extract was washed with water
  5. 5
    其他dried
  6. 6
    浓缩concentrated
  7. 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%.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06333323B1uspto-grants-2001_12