反应 #2171045

ord-6e9dccf8f1924bcca10f01ffe973992f

反应方程式

CC(=O)N(C)C
dimethylacetamide
O=P(Cl)(Cl)Cl
phosphorus oxychloride
[Na+].[OH-]
NaOH
c1ccc(Cc2cc3ccccc3[nH]2)cc1
2-benzylindole
CC(=O)c1c(Cc2ccccc2)[nH]c2ccccc12
titled compound
收率 53.0%
CC(=O)c1c(Cc2ccccc2)[nH]c2ccccc12
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. 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: US06716605B2uspto-grants-2004_04