반응 #9579

ord-6ce4ecf087dd4b5e9dfdb947815f2d30

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The crude product was triturated with water (200 mL)
  2. 2
    기타isolated by filtration
  3. 3
    세척washed with water
  4. 4
    기타dried
  5. 5
    기타The suspension was sonicated
  6. 6
    기타the resulting solid was isolated by filtration
  7. 7
    기타dried for four hours in a vacuum oven at 40° C.

실험 절차

7-Bromo-4-chloro-3-nitroquinoline (22.00 g, 76.52 mmol) was treated with (R)-2,2-dimethyl-1,3-dioxolane-4-methanamine (11.61 g, 114.8 mmol) according to the method described in Part A of Examples 152–156. The crude product was triturated with water (200 mL), isolated by filtration, washed with water, dried, and suspended in diethyl ether (100 mL). The suspension was sonicated, and the resulting solid was isolated by filtration, and dried for four hours in a vacuum oven at 40° C. to provide 25.84 g of (R)-(7-bromo-3-nitroquinolin-4-yl)-(2,2-dimethyl-1,3-dioxolan-4-ylmethyl)amine as a yellow solid, mp 136–137° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07091214B2uspto-grants-2006_08