反応 #74188

ord-f5a8391c359a43e2abd10f31d51a2ced

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度heated
  2. 2
    温度under reflux overnight
  3. 3
    その他Therefore, the reaction mixture was evaporated to a black gum
  4. 4
    その他the gum was absorbed onto silica
  5. 5
    その他purified by flash chromatography
  6. 6
    洗浄eluting with a gradient of hexane/ethyl acetate

実験手順

3-(2-chloro-acetyl)bicyclo[3.2.1]octane-2,4-dione (3.16 g, 14.7 mmol) and 4-chloro-thiobenzamide (2.53 g, 14.7 mmol) are mixed together in toluene (50 ml) and heated under reflux overnight. Therefore, the reaction mixture was evaporated to a black gum and the gum was absorbed onto silica and purified by flash chromatography eluting with a gradient of hexane/ethyl acetate to give 3-[2-(4-chloro-phenyl)thiazol-4-yl]bicyclo[3.2.1]octane-2,4-dione (2.6 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541594B2uspto-grants-2013_09