反应 #46362

ord-e387087c8a394279bd035d0d571cc60a

溶剂

反应条件

温度
90°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After cooling
  2. 2
    其他the reaction solution was partitioned between ethyl acetate and water
  3. 3
    洗涤The organic layer was washed with water, saturated brine
  4. 4
    其他dried
  5. 5
    其他evaporated
  6. 6
    其他The residue was chromatographed over silica gel
  7. 7
    洗涤eluting with a gradient of 10 to 50% ethyl acetate in hexane

实验过程

(S)-2-Aminomethyl-piperidine-1-carboxylic acid tert-butyl ester (1.14 g), and 2-chloro-6,7-difluoro-3-methylquinoxaline Teng et al PCT Int. Appl (2000), WO00/42026A1 20000720 (1.14 g) were dissolved in DMF (2 ml) and heated to 90° C. for 3 days under an atmosphere of argon. After cooling, the reaction solution was partitioned between ethyl acetate and water. The organic layer was washed with water, saturated brine, dried and evaporated. The residue was chromatographed over silica gel, eluting with a gradient of 10 to 50% ethyl acetate in hexane. The title compound was obtained as a pink foam (0.524 g), MH+ 393.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07741329B2uspto-grants-2010_06