반응 #55591

ord-8f19921b0ec84e5e914eba5e025e50e7

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The layers were separated
  2. 2
    추출the aqueous layer extracted with ether-ethyl acetate
  3. 3
    세척The combined extracts were washed with 10% aqueous sodium bicarbonate (NaHCO3)
  4. 4
    건조dried (MgSO4)
  5. 5
    여과filtered
  6. 6
    기타evaporated in vacuo

실험 절차

A solution of 24.4 g of Cyclobutane carbinol (prepared in Example 42A) in 570 ml of dry pyridine was stirred under argon at -10° C. and 81.0 g of tosyl chloride added in small portions. The reaction mixture was stirred at -10° C. to -0° C. for 4.5 hr, then poured into 1 liter of chilled 6 N HCl. The layers were separated and the aqueous layer extracted with ether-ethyl acetate. The combined extracts were washed with 10% aqueous sodium bicarbonate (NaHCO3), dried (MgSO4), filtered and evaporated in vacuo to yield 72.0 g of the title compound having the following physical characteristics:

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04220795uspto-grants-1980_09