HRID1481105
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 4-hydroxy-7-(4-fluoro-2-chloro-phenoxy)-isoquinoline-3-carboxylic acid ethyl ester (610 mg, 1.69 mmol) and NBS (331 mg, 1.86 mmol) in CH2Cl2 (17 mL) was refluxed for 3 h and then concentrated. Residue was triturate with acetone (15 mL). Solid was collected and dried to provide the title compound 540 mg (1.22 mmol) in 73% yield. 1H NMR (200 MHz) in CDCl3, δ ppm: 11.90 (s, 1H), 8.37 (d, J=8.8 Hz, 1H), 7.47 (m, 2H), 7.15 (m, 3H), 4.54 (br q, J=7.3 Hz, 2H), 1.49 (br t, J=7.3 Hz, 3H).
WORKUP
后处理
- temperaturewas refluxed for 3 h
- concentrationconcentrated
- customResidue was triturate with acetone (15 mL)
- customSolid was collected
- customdried