반응 #1729285

ord-a1f62cc170df48eb81901dd9ad9550c6

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the organic phase was separated off
  2. 2
    세척washed in succession with water (4×150 ml) and aqueous FeSO4 solution (4×150 ml)
  3. 3
    기타The organic phase was separated off
  4. 4
    건조dried over Na2SO4
  5. 5
    여과filtered off
  6. 6
    기타The solvent was removed in vacuo
  7. 7
    기타without being purified further

실험 절차

KCN (0.17 mol) and morpholine (14.7 g, 0.17 mol) were added to a solution of 1,4-dioxa-spiro[4.5]decane-8-carboxaldehyde (0.141 mol) in a mixture of ethanol (141 ml) and water (70 ml), and stirring was carried out for 72 h at 25° C. After addition of ethyl acetate (700 ml), the organic phase was separated off and washed in succession with water (4×150 ml) and aqueous FeSO4 solution (4×150 ml). The organic phase was separated off and dried over Na2SO4 and then filtered off. The solvent was removed in vacuo, and the product was used in the next stage without being purified further.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08119633B2uspto-grants-2012_02