反应 #607468

ord-68c1ffa6ddc34379bd6fe87116192aab

反应方程式

CCc1nc2ccccc2c(=O)n1CCO
2-ethyl-3-(2-hydroxyethyl)quinazoline-4 (3H)-one
O=S(Cl)Cl
thionyl chloride
ClC(Cl)Cl
chloroform
CCc1nc2ccccc2c(=O)n1CCCl
3-(2-chloroethyl)-2-ethylquinazoline-4 (3H)-one
收率 32.8%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction medium was heated
  2. 2
    温度to reflux
  3. 3
    其他the reaction, which
  4. 4
    workup.ADDITIONwere added
  5. 5
    其他to precipitate the product
  6. 6
    过滤filtered
  7. 7
    洗涤washed with two portions of hexane
  8. 8
    其他dried

实验过程

2-ethyl-3-(2-hydroxyethyl)quinazoline-4 (3H)-one (5.00 g; 22.91 mmol) and thionyl chloride (1.672 mL, 22.91 mmol) were added to a 150 mL reactor, together with 60 mL of chloroform. The reaction medium was heated to reflux and for completing the reaction, which was accompanied through CG/MS. After the end of the reaction, 100 mL of hexane were added and the solution was agitated at room temperature in order to precipitate the product. The resulting suspension was vacuum filtered, washed with two portions of hexane and dried, yielding 3-(2-chloroethyl)-2-ethylquinazoline-4 (3H)-one as a white solid (1.78 g; 7.52 mmol; yield: 32.8%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09326984B2uspto-grants-2016_05