反応 #607468

ord-68c1ffa6ddc34379bd6fe87116192aab

反応方程式

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
収率 32.8%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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%).

出典

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