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
139 g (2 mols) of hydroxylamine hydrochloride are dissolved in 200 ml of water; there are then added 408 g (2 mols) of allylbicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic anhydride (produced according to Example 1 of the U.S. Pat. No. 3,105,839), and 160 g of 50% aqueous sodium hydroxide solution are subsequently introduced dropwise with vigorous stirring. The mixture is afterwards refluxed for 1 hour; the water and traces of oily constituents are distilled off, the residue is taken up in toluene, the sodium chloride is filtered off, and the toluene is removed in a rotary evaporator at 150° C. and 2000 Pa. There remain 402.6 g of the product (91.5% of theory) in the form of a light-brown viscous liquid having a viscosity of 1.28 Pa.s at 80° C.
WORKUP
后处理
- customproduced
- temperatureThe mixture is afterwards refluxed for 1 hour
- distillationthe water and traces of oily constituents are distilled off
- filtrationthe sodium chloride is filtered off
- customthe toluene is removed in a rotary evaporator at 150° C.
- customat 80° C.