反応 #595322
ord-4f96d1fe87c14ca99ef2063384456be5
反応方程式
potassium 1-allylcyclopropane-1-sulfonate
thionyl chloride
→
crude product
1-allylcyclopropane-1-sulfonyl chloride
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他The volatiles evaporated under reduced pressure
- 2抽出the residue extracted with CH2Cl2 (50 ml)
- 3洗浄The extract was washed with water
- 4乾燥dried (MgSO4)
- 5その他evaporated
実験手順
A solution of potassium 1-allylcyclopropane-1-sulfonate (3.44 g, 17.2 mmol), thionyl chloride (10 ml) and DMF (5 drops) was refluxed at 60° C. for 16 h. The volatiles evaporated under reduced pressure and the residue extracted with CH2Cl2 (50 ml). The extract was washed with water, dried (MgSO4) and evaporated to obtain the crude product as yellow gummy oil which was washed with hexane and used in the next reaction without further purification (2.7 g, 15 mmol, 87%). 1HNMR (300 MHz, CDCl3): δ 5.728 (m, 1H), 5.191 (t, 2H), 2.9 (d, 2H), 0.756 (m, 2H), 0.322 (m, 2H).