反应详情

温度

-20 °C

To a solution of the product of Example 14 (2.0 g, 4.58 mmol) stirring in methanol (50 mL) at ambient temperature was added methanolic hydrochloric acid (10 mL of a saturated solution). The reaction mixture was then concentrated to 20 mL and cooled to -20° C. for several hours. Filtration gave 0.62 g of the desired product as a white powder: 1H-NMR (CDCl3, 300 MHz) consistent with structure; MS (FD) m/e 437 (M+ -hydrochloric acid); Anal. Calc'd. for: C, 76.01; H, 6.80; N, 2.96. Found: C, 75.95; H, 6.76; N, 2.98.

1. concentrationThe reaction mixture was then concentrated to 20 mL
2. filtrationFiltration