HRID1030369
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
- 120 °C
PROCEDURE
实验过程
A mixture of 9.6 g of ethyl 3-[4-(6-acetoxy-2,5,7,8-tetramethylchroman-2-ylmethoxy)phenyl]-2-chloropropionate (prepared as described in Preparation 51), 1.8 g of thiourea and 11 ml of sulfolane was heated for 3.5 hours at 120° C. under a nitrogen stream. 100 ml of ethylene glycol monomethyl ether and 70 ml of 10% w/v aqueous hydrochloric acid were then added to the reaction mixture, after which it was heated under reflux for 12 hours. The product was then purified as described in Example 27, to give the title compound. The melting point and nuclear magnetic resonance spectrum of this compound accorded with those of the compound obtained in Example 27(b).
WORKUP
后处理
- additionwere then added to the reaction mixture
- temperatureafter which it was heated
- temperatureunder reflux for 12 hours
- customThe product was then purified