反応 #73509

ord-8127a537d4e242ff81ca2df85f83c037

溶媒

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONare added portionwise, at 0° C.
  2. 2
    洗浄washed with water (1 L), saturated NaHCO3 solution (1 L) and brine (1 L)
  3. 3
    乾燥dried over Na2SO4
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated under reduced pressure

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541455B2uspto-grants-2013_09