反应 #595322

ord-4f96d1fe87c14ca99ef2063384456be5

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The volatiles evaporated under reduced pressure
  2. 2
    萃取the residue extracted with CH2Cl2 (50 ml)
  3. 3
    洗涤The extract was washed with water
  4. 4
    干燥dried (MgSO4)
  5. 5
    其他evaporated

实验过程

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).

来源

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