| 摘要 |
<p>1304667 Preparation of cyclopropylamine GULF RESEARCH & DEVELOPMENT CO 19 April 1971 [19 May 1970] 26886/71 Addition to 1257097 Heading C2C A process for the preparation of cyclopropylamine comprises effecting amidation of C 1-4 alkyl cyclopropanecarboxylate by reaction thereof with gaseous ammonia at a temperature within the range from 80‹ to 115‹ C. in the absence of water and in the presence of 0À1 to 0À3 moles of alkali metal alkoxide and 40 to 80 ml. of an alkanol per mole of alkyl cyclopropanecarboxylate, the ammonia being present in a ratio of from 1 to 3 moles per mole of alkyl cyclopropanecarboxylate to obtain a reaction product mixture containing cyclopropanecarboxamide; distilling the reaction product mixture to obtain a distillate residue containing cyclopropanecarboxamide, mixing the distillation residue with water and mineral acid to obtain an aqueous solution phase and an organic liquid phase; mixing the aqueous solution phase with an aqueous solution of an alkali metal hypochlorite to yield a homogeneous solution reaction mixture and reacting said mixture with an aqueous alkali metal hydroxide solution, the addition of alkali metal hydroxide solution being made prior to raising the temperature above 40‹ C. to yield a product mixture containing cyclopropylamine; and distilling the product mixture to obtain an aqueous solution of cyclopropylamine.</p> |
