反応 #607467

ord-7f52c776ce9240d6859264ef7c924bcb

反応方程式

CCc1nc2ccccc2c(=O)o1
2-ethyl-4H-3,1-benzoxazin-4-one
NCCO
monoethanolamine
CCc1nc2ccccc2c(=O)n1CCO
2-ethyl-3-(2-hydroxyethyl)quinazoline-4 (3H)-one

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The heating element was then removed
  2. 2
    その他(end of the reaction)
  3. 3
    workup.ADDITION100 mL were added to the reaction medium
  4. 4
    抽出the mixture was extracted with three portions of 25 mL of ethyl acetate
  5. 5
    その他The organic phase was separated
  6. 6
    乾燥dried with magnesium sulfate
  7. 7
    その他spin dried

実験手順

1 g of 2-ethyl-4H-3,1-benzoxazin-4-one was added to 10 mL of monoethanolamine and the mixture was heated to 100° C. for 40 minutes. The heating element was then removed and the reaction medium was kept under agitation for about eight hours (end of the reaction). 100 mL were added to the reaction medium and the mixture was extracted with three portions of 25 mL of ethyl acetate. The organic phase was separated, and dried with magnesium sulfate and spin dried, yielding the 2-ethyl-3-(2-hydroxyethyl)quinazoline-4 (3H)-one compound as a yellowish oil, which solidified when left to rest at room temperature, which was used in the next stage, with no purification.

出典

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