反応 #50001

ord-a7ad4b452cd840e4b80e1f788cd0e5ae

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度under reflux for 5 hours
  2. 2
    温度After cooling
  3. 3
    その他the resulting crystals were separated off
  4. 4
    その他They were dried at 50° C. in vacuo
  5. 5
    その他purified by column chromatography

実験手順

A solution of 6 g 7-amino-2,4-dichloro-6-fluoro-benzothiazole and 4.3 g 3,4,5,6-tetrahydrophthalic anhydride in 50 ml acetic acid was heated under reflux for 5 hours. After cooling, the reaction solution was poured into 200 ml ice-water and the resulting crystals were separated off. They were dried at 50° C. in vacuo and then purified by column chromatography. Yield: 6.6 g=70% of theory m.p.: 139°-141° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05424443uspto-grants-1995_06