asynthesisoftropinone托品酮合成(編輯修改稿)
2024-09-26 16:29 本頁面
【文章內(nèi)容簡(jiǎn)介】 f the dipiperonylidene derivative serves as a means of detection of the merest traces of tropinone, and the test may be applied in the following manner. A solution which it is suspected contains the base may first be acidified and evaporated in a vacuum in order to remove possible volatile neutral impurities, such as acetone. Alcohol, an excess of piperonal, and potassium hydroxide are then added, and the solution heated on the steambath for two or three minutes and then poured into ether. The ethereal solution is washed with water and separated, and then agitated with a little dilute hydrochloric acid. If tropinone is present, the hydrochloride of the derivative is so obtained in a crystalline condition. Synthesis of Tropinone from succindialdehyde, methylamine, and acetone. In this reaction, which has not yet been sufficiently investigated, it seemed that the tropinone could only be detected after the expiration of a brief period from the time of addition of the methylamine. If the reaction mixture was allowed to remain overnight, other basic ketones were obtained which condensed with piperonal and interfered with the recognition of the desired product. Succindialdoxime (7g) suspended in water (30ml) was converted into succindialdehyde by means of nitrous fumes generated from nitric acid () and arsenious oxide according to the method developed by Harries (Ber., 1901,34,1494).Water (50ml) was then added, and the nitrous and nitric acids neutralized by means of an excess of precipitated calcium carbonate. After the addition of acetone (5g) , and then methylamine() dissolved in water (20ml) , the mixture was allowed to remain during half an hour. The solution was acidified with hydrochloric acid and tested for tropinone by the method described above. The small quantity of the crystalline hydreochloride was collected, treated with a little aqueous ammonia, and the base crystallized from ethyl acetate. The yellow needles melted at 214, and at the same temperature when mixed with a specimen of dipiperonylideropinone. The colour reactions of the two specimens in concentrated sulphuric acid were identical. Synthesis of Tropinone from Succindialdehyde, Methylamine, and Ethyl Acetonedicarboxylate ??Succindialdehyde (1g) and ethyl acetonedicarboxylate () were dissolved in alcohol (20ml) , and, after cooling in icewater , a solution of methylamine () in alcohol (10ml) was gradually added during an hour. After remaining overnight at the ordinary temperature, the alcohol was removed by distillation in a vacuum, and the residue boiled with dilute sulphuric a
研究報(bào)告相關(guān)推薦
鄂ICP備17016276號(hào)-1