HRID4848
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 4.5 g (0.015 mole) of 2-(2-chloroethyl)-2,3-dihydro-2,4-dimethylpyrido[3,2-f]-1,4-oxazepin-5(4H)-one hydrochloride in 15 ml of methanol was added 40 ml of dimethylamine. The flask was sealed tightly and left standing at room temperature for 8 days. The methanol and dimethylamine were removed by rotary evaporation (70° C.; 30 mm). The residue was taken up in 150 ml of chloroform, washed with 2×50 ml dil aqueous sodium hydroxide, dried over anhydrous sodium sulfate, filtered and concentrated by rotary evaporation (70° C.; 30 mm). The syrupy residue was treated with hydrogen chloride in isopropyl alcohol, which afforded 3.5 g (67%) of white crystals, m.p. 188°-90° C.
WORKUP
后处理
- customThe flask was sealed tightly
- waitleft
- customThe methanol and dimethylamine were removed by rotary evaporation (70° C.; 30 mm)
- washwashed with 2×50 ml dil aqueous sodium hydroxide
- dry with materialdried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated by rotary evaporation (70° C.; 30 mm)
- additionThe syrupy residue was treated with hydrogen chloride in isopropyl alcohol, which