反応 #2000409

ord-0aa7901b78364218a7d604840122b8ef

溶媒

反応条件

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

後処理

  1. 1
    workup.ADDITIONThe mixture was mixed
  2. 2
    その他to remove water
  3. 3
    その他formed during cyclization
  4. 4
    その他This solid was taken forward without further purification

実験手順

To a 20 mL scintillation vial containing ethyl 3-oxo-3-(1,4-dioxaspiro[4.5]decan-8-yl)propanoate (Int-5d, 11.7 mmol, 3.00 g) was added 3-amino-1H-pyrazole (11.7 mmol, 973 mg). The mixture was mixed and heated neat at 100° C. for 3 hours. The resulting off-white solid was taken up in EtOH (100 mL) and reduced in vacuo to remove water formed during cyclization. This solid was taken forward without further purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08609675B2uspto-grants-2013_12