反応 #7721

ord-7db9ee3861144166bfa97d305c987b83

溶媒

反応条件

温度
130°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After cooling
  2. 2
    その他evaporated
  3. 3
    その他an off-white solid formed
  4. 4
    ろ過the solid filtered off
  5. 5
    洗浄washed with water
  6. 6
    洗浄The solid was then washed with hexane
  7. 7
    その他dried under high vacuum

実験手順

7-Fluoro-3H-quinazolin-4-one: A mixture of 2-amino-4-fluorobenzoic acid (14.6 g, 94 mmol) and formamidine acetate (19.6 g, 18.8 mmol) in 2-methoxyethanol (110 mL) was heated at 130° C. for 18 h. After cooling, the mixture was half evaporated and an off-white solid formed. The mixture was diluted with ammonia (25%, 10 mL in 90 mL water) and the solid filtered off and washed with water. The solid was then washed with hexane and dried under high vacuum to afford the title compound (12.5 g, 81%) as an off-white solid. MS: m/e=165.2 (M+H+).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07087612B2uspto-grants-2006_08