تفاعل #9579

ord-6ce4ecf087dd4b5e9dfdb947815f2d30

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe crude product was triturated with water (200 mL)
  2. 2
    أخرىisolated by filtration
  3. 3
    غسيلwashed with water
  4. 4
    أخرىdried
  5. 5
    أخرىThe suspension was sonicated
  6. 6
    أخرىthe resulting solid was isolated by filtration
  7. 7
    أخرىdried for four hours in a vacuum oven at 40° C.

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07091214B2uspto-grants-2006_08