反応 #9579

ord-6ce4ecf087dd4b5e9dfdb947815f2d30

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The crude product was triturated with water (200 mL)
  2. 2
    その他isolated by filtration
  3. 3
    洗浄washed with water
  4. 4
    その他dried
  5. 5
    その他The suspension was sonicated
  6. 6
    その他the resulting solid was isolated by filtration
  7. 7
    その他dried for four hours in a vacuum oven at 40° C.

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091214B2uspto-grants-2006_08