反応 #73435

ord-3977ce71efee440385264c98363f3da1

反応条件

温度
79°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction is cooled to room temperature
  2. 2
    洗浄The organic layer is washed with 500 mL of water
  3. 3
    その他to remove the acid
  4. 4
    乾燥The organic layer is dried (sodium sulfate)
  5. 5
    濃縮concentrated to an oil (352 mg)

実験手順

(5-Cyclopropyl-isoxazol-3-yl)-carbamic acid phenyl ester (0.25 g, 1.024 mmol) is dissolved in AcOH (7.31 mL) and NCS (0.205 g, 1.53 mmol) is added and the reaction is heated to 79° C. for 2 hours. The reaction is cooled to room temperature and diluted with water and ethyl acetate. The organic layer is washed with 500 mL of water to remove the acid. The organic layer is dried (sodium sulfate) and concentrated to an oil (352 mg) to obtain the title compound that is used without further purification. MS (ESI) m/z 279.00 (M+1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541432B2uspto-grants-2013_09