반응 #654057

ord-d0c80c34be8242cfb1bf393155c62d2b

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction is quenched by addition of 50 mL of water
  2. 2
    기타the THF is removed under reduced pressure
  3. 3
    여과The precipitate is collected by filtration
  4. 4
    기타recrystallized from methanol

실험 절차

Sodium triacetoxyborohydride (1.2 g, 5.9 mmol) is added to a solution of 3-oxo-3,4-dihydro-2H-benzo[1,4]-oxazine-6-carbaldehyde (0.5 g, 2.8 mmol) and 4-(piperazin-1-yl)-benzenesulfonamide (0.17 g, 3.1 mmol) in 20 mL of THF. The mixture is stirred at room temperature overnight. The reaction is quenched by addition of 50 mL of water, and the THF is removed under reduced pressure. The precipitate is collected by filtration and recrystallized from methanol to give 0.05 g (4% yield) of 4-[4-(3-oxo-3,4-dihydro-2H-benzo[1,4]oxazin-6-ylmethyl)-piperazin-1-yl]-benzenesulfonamide; mp 150-153° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06177422B1uspto-grants-2001_01