HRID929505
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
PROCEDURE
实验过程
Intermediate 41 (2.02 g, 5.0 mmol) was treated with 1M HCl in methanol (35 mL) and refluxed for 3 hours. The solvent was evaporated and the residue diluted with 1N NaOH. The resulting precipitate was removed by filtration and further dried under high vacuum to give intermediate 42 (1.35 g, 89%) as a white solid: Mp 169-173° C. 1H NMR (500 MHz, DMSO-d6) δ 8.49 (s, 1H), 7.46 (d, J=9.0 Hz, 2H), 7.21 (d, J=8.6 Hz, 2H), 6.15 (d, J=7.7 Hz, 1H), 3.55-3.45 (m, 1H), 2.89 (td, J=12.8, 3.5 Hz, 2H), 2.49-2.45 (m, 2H), 2.13 (s, 1H), 1.74 (dd, J=12.4, 2.4 Hz, 2H), 1.21 (dq, J=11.7, 3.7 Hz, 2H). HRMS calculated for C13H16F3N3O2−H+ 302.1117. found (ESI(−), [M−H]) 302.1114.
WORKUP
后处理
- temperaturerefluxed for 3 hours
- customThe solvent was evaporated
- additionthe residue diluted with 1N NaOH
- customThe resulting precipitate was removed by filtration
- customfurther dried under high vacuum