HRID568586

反应详情

EQUATION

反应方程式

HRID 568586 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customproduced
  2. temperatureThe mixture is afterwards refluxed for 1 hour
  3. distillationthe water and traces of oily constituents are distilled off
  4. filtrationthe sodium chloride is filtered off
  5. customthe toluene is removed in a rotary evaporator at 150° C.
  6. customat 80° C.