CAS: 504-02-9; Cyclohexane-1,3-Dione

上下游产品

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4-乙酰基-5-羰基己酸甲酯置于sodium Methylate,盐酸体系中,用 水 作为反应溶剂,化学反应 1.0H,以93.1%的收率获得产物1,3-环己二酮
参考文献:一种1,3环己二酮的制备工艺
标题:一种1,3环己二酮的制备工艺
摘要:本发明公开了一种制备1,3‑环己二酮的方法:1)将乙酰丙酮和催化剂溶于溶剂中,将丙烯酸酯加入恒压滴液漏斗中向反应体系中滴加丙烯酸酯.滴加完毕加热到60oc‑80oc继续反应0.5‑1H;2)反应结束后,降温到40°C,并加入固体缩合剂将反应液升温至40‑50°C,继续反应1‑1.5H,减压浓缩除去溶剂以及反应产生的乙酸甲酯等低沸点副产物,然后加入少量水,用盐酸(1.1‑1.2当量)调节ph值到1‑2,冷却析出产品,离心,用少量冰水淋洗,然后用乙酸乙酯进行打浆处理,过滤,烘干得到1,3‑环己二酮产品.

专利信息

专利号:US-6995289-B2
优先权日:2000-08-02
标题 :Process for synthesis of alpha, beta-unsaturated ketones
发明人：PATEL IAN; HOPES PHILIP
权利人:ASTRAZENECA AB
摘要:A method for the synthesis of an α,β-unsaturated ketone useful for making substituted 1,4-dihydropyridines is described by reacting an aldehyde with pyrrolidine and then adding a ketone followed by trifluoroacetic acid at low temperature. The synthesis is used in a process for making substituted 1,4-dihydropyridines wherein a vinylogous amide is prepared by reacting a 1,3-cyclohexanedione with a phenylethylamine. The α,β-unsaturated ketone can be reacted with a vinylogous amide to form a 1,5-diketone which can be converted to a substituted 1,4-dihydropyridine.

专利号:US-11008285-B2
优先权日:2017-03-27
标 题 :Process for synthesis of mesotrione
发明人：GHARDA KEKI HORMUSJI; MATHUR SUCHET SARAN; JAIN NANDKUMAR JANARDAN; SATHE SHEKHAR VISHWANATH; DAMANIA PRAGNESH DALPATRAM
权利人:GHARDA CHEMICALS LTD
摘要:The present disclosure relates to a process for synthesis of mesotrione. The process comprises reacting 4-toluene sulfonyl chloride with alkali metal sulphite and alkali metal bicarbonate to obtain alkali metal toluene-4-sulfinate. The alkali metal toluene-4-sulfinate is reacted with alkali metal salt of monochloroacetic acid to obtain 4-methylsulfonyl toluene. Further, 4-methylsulfonyl toluene is nitrated to obtain 2-nitro-4-methylsulfonyl toluene. 2-nitro-4-methylsulfonyl toluene is oxidized and then halogenated to obtain 2-nitro-4-methylsulfonylbenzoyl halide. 2-nitro-4-methylsulfonylbenzoyl halide is reacted with alkali metal salt of 1,3-cyclohexanedione to obtain 3-(2-Nitro-4-methylsulfonylbenzoyloxy)cyclohexen-1-one which is reacted with base, a third fluid medium and cyanide ion source to obtain an amorphous mesotrione. The present disclosure also discloses the steps of converting the amorphous mesotrione to crystalline mesotrione having purity greater than 99%. The process of the present disclosure for preparing mesotrione is rapid, economic, and environment friendly.

专利号:US-4045452-A
优先权日:1974-03-13
标题 :Steroid total synthesis process utilizing a cyanoalkyl A-ring precursor
发明人：COHEN NOAL; ROSENBERGER MICHAEL; SAUCY GABRIEL
权利人:HOFFMANN LA ROCHE
摘要:A multi-step, stereospecific total synthesis of steroids utilizing intermediates having a cyanoalkyl A-ring precursor is disclosed. The initial starting materials for this process are the relatively inexpensive and commercially available reagents γ-butyrolactone and sodium cyanide. The process is suitable for the preparation of racemic or optically active, medicinally valuable steroids, particularly 19-norsteroids. It is a feature of this process that conditions employed during the multiple step synthesis are selected so as to retain the normally labile nitrile group even during hydrogenation and hydrolysis steps. In this manner, it is possible to employ the nitrile group as an A-ring precursor without resorting to protective groups as wasl heretofore found necessary in previous steroid total synthesis processes.

专利号:US-4105676-A
优先权日:1975-12-22
标题 :Steroid total synthesis process utilizing a cyanoalkyl a-ring precursor
发明人：COHEN NOAL; ROSENBERGER MICHAEL; SAUCY GABRIEL
权利人:HOFFMANN LA ROCHE
摘要:A multi-step, stereospecific total synthesis of steroids utilizing intermediates having a cyanoalkyl A-ring precursor is disclosed. The initial starting materials for this process are the relatively inexpensive and commercially available reagents γ-butyrolactone and sodium cyanide. The process is suitable for the preparation of racemic or optically active, medicinally valuable steroids, particularly 19-norsteroids. It is a feature of this process that conditions employed during the multiple step synthesis are selected so as to retain the normally labile nitrile group even during hydrogenation and hydrolysis steps. In this manner, it is possible to employ the nitrile group as an A-ring precursor without resorting to protective groups as was heretofore found necessary in previous steroid total synthesis processes.

专利号:US-3965138-A
优先权日:1974-03-13
标 题:Steroid total synthesis process utilizing a cyanoalkyl A-ring precursor
发明人：COHEN NOAL; ROSENBERGER MICHAEL; SAUCY GABRIEL
权利人:HOFFMANN LA ROCHE
摘要:A multi-step, stereospecific total synthesis of steroids utilizing intermediates having a cyanoalkyl A-ring precursor is disclosed. The initial starting materials for this process are the relatively inexpensive and commercially available reagents γ-butyrolactone and sodium cyanide. The process is suitable for the preparation of racemic or optically active, medicinally valuable steroids, particularly 19-norsteroids. It is a feature of this process that conditions employed during the multiple step synthesis are selected so as to retain the normally labile nitrile group even during hydrogenation and hydrolysis steps. In this manner, it is possible to employ the nitrile group as an A-ring precursor without resorting to protective groups as was heretofore found necessary in previous steroid total synthesis processes.

专利号:US-3991084-A
优先权日:1970-08-26
标题 :Steroid total synthesis process utilizing a cyanoalkyl A-ring precursor
发明人：COHEN NOAL; ROSENBERGER MICHAEL; SAUCY GABRIEL
权利人:HOFFMANN LA ROCHE
摘要:A multi-step, stereospecific total synthesis of steroids utilizing intermediates having a cyanoalkyl A-ring precursor is disclosed. The initial starting materials for this process are the relatively inexpensive and commercially available reagents γ-butyrolactone and sodium cyanide. The process is suitable for the preparation of racemic or optically active, medicinally valuable steroids, particularly 19-norsteroids. It is a feature of this process that conditions employed during the multiple step synthesis are selected so as to retain the normally labile nitrile group even during hydrogenation and hydrolysis steps. In this manner, it is possible to employ the nitrile group as an A-ring precursor without resorting to protective groups as was heretofore found necessary in previous steroid total synthesis processes.