반응 #73509

ord-8127a537d4e242ff81ca2df85f83c037

용매

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONare added portionwise, at 0° C.
  2. 2
    세척washed with water (1 L), saturated NaHCO3 solution (1 L) and brine (1 L)
  3. 3
    건조dried over Na2SO4
  4. 4
    여과filtered
  5. 5
    농축concentrated under reduced pressure

실험 절차

To a mixture of 17.3 mL (165 mmol) of tert-butylamine and 69 mL (495 mmol) of TEA in 330 mL of DCM are added portionwise, at 0° C., 35 g (165 mmol) of 6-chloropyridine-3-sulfonyl chloride. After stirring for 2 hours at 0° C., the reaction medium is taken up in 600 mL of DCM, washed with water (1 L), saturated NaHCO3 solution (1 L) and brine (1 L), dried over Na2SO4, filtered and concentrated under reduced pressure. 32.4 g of N-tertbutyl-6-chloropyridine-3-sulfonamide are obtained in the form of a white solid.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541455B2uspto-grants-2013_09