HRID1817366
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
- 90 °C
PROCEDURE
实验过程
A solution of ethyl 3,4-bis(acetyloxy)-6-(3-chloro-4-fluorobenzyl)-5-oxo-5,6,7,8-hexahydro-2,6-naphthyridine-1-carboxylate (1.00 g, 2.09 mmol; Example 12, step 8) and lithium hydroxide (0.70 g, 16.70 mmol) in a mixture of THF-methanol-water (30 mL, 1:1:1 by volume) was heated under reflux in an oil bath at 90° C. overnight. The product mixture was acidified and concentrated under vacuum. The residue was triturated with diethyl ether. The solid precipitated was filtered and washed with ether to provide the titled compound. ES MS M+1=367.
WORKUP
后处理
- temperaturewas heated
- concentrationconcentrated under vacuum
- customThe residue was triturated with diethyl ether
- customThe solid precipitated
- filtrationwas filtered
- washwashed with ether