反应详情

A stirred solution of 1-chloro-6-methyl-5-nitroisoquinoline (1.2 g, 5.4 mmol) and sodium methoxide (0.6 g, 95%, 11 mmol) in methanol (20 mL) in a sealed-tube was heated to 80° C. for 2 h, cooled to room temperature and partitioned between ethyl acetate (3×30 mL) and water (50 mL). The combined organic extracts were washed (water, brine), dried (sodium sulfate) and concentrated in vacuo to give the product as a beige solid (0.87 g, 74%). A sample recrystallised from ethanol gave mp 94° C.; Found: C, 60.45; H, 4.58; N, 12.74%. C11H10N2O3 requires C, 60.55; H, 4.62; N, 12.83%.

1. custompartitioned between ethyl acetate (3×30 mL) and water (50 mL)
2. washThe combined organic extracts were washed (water, brine)
3. dry with materialdried (sodium sulfate)
4. concentrationconcentrated in vacuo