HRID1794519
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
- 200 °C
PROCEDURE
实验过程
Compound 86 was treated with Pyridine HCl (5 g) and heated to 200° C. After 1 hr, the reaction was cooled and diluted with water. The aqueous layer was extracted with EtOAc, dried, and the product was purified by column chromatography (eluent 25% EtOAc/hex) to give a solid (0.12 g, 13%): Mp=152–154° C.; 1H NMR (DMSO-d6) δ 10.01 (br s, 1 H), 7.77 (d, 2 H, J=8.9 Hz), 7.32–7.25 (m, 3 H), 6.91 (d, 2 H, J=8.9 Hz); MS 245 [M−H]−
WORKUP
后处理
- temperaturethe reaction was cooled
- extractionThe aqueous layer was extracted with EtOAc
- customdried
- customthe product was purified by column chromatography (eluent 25% EtOAc/hex)