반응 #160576

ord-e4e738bec7e5404fb954877e0388aa79

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The volatiles evaporated under reduced pressure
  2. 2
    추출the residue extracted with CH2Cl2 (50 ml)
  3. 3
    세척The extract was washed with water
  4. 4
    건조dried (MgSO4)
  5. 5
    기타evaporated

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08829052B2uspto-grants-2014_09