반응 #64962

ord-b43a0c6fcedb452497400e46b1e3cb3d

용매

반응 조건

온도
90°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The sodium chloride which has precipitated out
  2. 2
    workup.DISSOLUTIONis dissolved with water
  3. 3
    기타the organic phase is separated off
  4. 4
    건조dried over K2CO3
  5. 5
    농축concentrated
  6. 6
    workup.DISTILLATIONthe residue is distilled

실험 절차

131 g (0.686 mol) of N-(1,1-dimethoxyprop-2-yl)urethane are added dropwise to 25 g of sodium hydride (80% strength) in 700 ml of absolute toluene at 90° C. When the evolution of hydrogen has ended, 61.2 g (0.8 mol) of allyl chloride are added dropwise at 90° C and the mixture is stirred overnight at 90° C. The sodium chloride which has precipitated out is dissolved with water, the organic phase is separated off, dried over K2CO3 and concentrated and the residue is distilled.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05416096uspto-grants-1995_05