反応 #595322

ord-4f96d1fe87c14ca99ef2063384456be5

反応方程式

C=CCC1(S(=O)(=O)[O-])CC1.[K+]
potassium 1-allylcyclopropane-1-sulfonate
O=S(Cl)Cl
thionyl chloride
C=CCC1(S(=O)(=O)Cl)CC1
crude product
C=CCC1(S(=O)(=O)Cl)CC1
1-allylcyclopropane-1-sulfonyl chloride

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The volatiles evaporated under reduced pressure
  2. 2
    抽出the residue extracted with CH2Cl2 (50 ml)
  3. 3
    洗浄The extract was washed with water
  4. 4
    乾燥dried (MgSO4)
  5. 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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09095581B2uspto-grants-2015_08