HRID30974
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
To a solution of 5h (0.097 g, 0.025 mmol) in conc H2SO4 (0.65 mL) cooled on ice bath was added conc HNO3 (0.10 mL). After stirring 30 min at 0° C., the reaction mixture was poured onto crushed ice (1.5 g). The resulting precipitate was collected by filtration to give 5i (0.091 g, 85%) as a yellow solid. 1H NMR (400 MHz, D6-DMSO) δ 13.90 (s, 1 H), 8.57 (d, J=2.8 Hz, 1 H), 8.49 (dd, J=9.2, 2.8 Hz, 1 H), 7.82 (d, J=8.8 Hz, 1 H), 4.11 (t, J=6.8 Hz, 2 H), 3.23 (m, 2 H), 1.61 (m, 2 H), 1.21 (d, J=8 Hz, 6 H), 0.93 (d, J=8 Hz, 6 H). MS (ESI+) m/e 450 [M+H]+.
WORKUP
后处理
- additionthe reaction mixture was poured
- filtrationThe resulting precipitate was collected by filtration