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
To a solution of 2,4-dichloro-6-methyl-1,3,5-triazine (190 g, 1159 mmol) in DMF (1500 mL) was added (4-methoxyphenyl)methanamine (159 g, 1159 mmol) slowly in 15 min while the temperature was controlled below 20° C. This was followed by the addition of N-ethyl-N-isopropylpropan-2-amine (222 mL, 1274 mmol) slowly over 15 min. After the completion of the reaction, EtOAc (2000 mL) was added and the mixture was washed with dilute brine (200 mL saturated NaCl plus 500 mL water), water (500 mL), saturated NH4Cl (250 mL), and finally water (250 mL). The organic layer was concentrated to afford 4-chloro-N-(4-methoxybenzyl)-6-methyl-1,3,5-triazin-2-amine as a solid (290.5 g, 1097 mmol, 95% yield). m/z 265.2 (M+H).
WORKUP
后处理
- customwas controlled below 20° C
- additionwas added
- washthe mixture was washed with dilute brine (200 mL saturated NaCl plus 500 mL water), water (500 mL), saturated NH4Cl (250 mL), and finally water (250 mL)
- concentrationThe organic layer was concentrated