HRID651599
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
7-Methoxynaphthalene-2-sulfonic acid [1-(1-chloro-isoquinolin-7-ylmethyl)-2-oxopyrrolidin-3-(S)-yl]amide (0.07 g, 0.14 mmol), prepared as described in EXAMPLE 1, Part K, is treated with dioxane (1 mL) and 10% aq. NaOH (3 mL) and heated to reflux for 48 hours. The reaction was cooled, acidified with 1 N HCl and extracted with CH2Cl2. The organic layer is separated, dried and concentrated. The residue is purified by column chromatography eluting with 2.5% MeOH/CH2Cl2. The product fractions are collected, concentrated and precipitated with dilute HCl/ether to yield the title compound (0.041 g, 0.086 mmol).
WORKUP
后处理
- temperatureheated
- temperatureto reflux for 48 hours
- temperatureThe reaction was cooled
- extractionextracted with CH2Cl2
- customThe organic layer is separated
- customdried
- concentrationconcentrated
- customThe residue is purified by column chromatography
- washeluting with 2.5% MeOH/CH2Cl2
- customThe product fractions are collected
- concentrationconcentrated
- customprecipitated with dilute HCl/ether