HRID1409743
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
8-(5-Chloropyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4.5]decane (4.2 g) is dissolved in 6 M HCl (50 mL) and stirred at r.t. for 60 h. The solution is cooled in an ice bath and 4 M NaOH (90 mL) is added in portions to make the solution strongly basic (pH ˜14). The mixture is extracted with dichloroemethane (2×200 mL) and the combined dichloromethane layers are dried over Na2SO4, filtered and concentrated to yield the title compound. LC (method 21): tR=4.21 min; Mass spectrum (APCI): m/z=212 [M+H]+.
WORKUP
后处理
- temperatureThe solution is cooled in an ice bath
- extractionThe mixture is extracted with dichloroemethane (2×200 mL)
- dry with materialthe combined dichloromethane layers are dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated