5-[1-羟基-2-(2,4,5-三氟苯基)亚乙基]-2,2-二甲基-1,3-二氧六环-4,6-二酮合成路线 (共 12 条)
反应条件
1: 4-methyl-morpholine / ethyl acetate / 6 h / Reflux 2: acetic acid / 5 h / Reflux View Scheme
参考文献
DR. REDDY'S LABORATORIES LTD.; DR. REDDY'S LABORATORIES, INC.; BANDICHHOR, Rakeshwar; GUDIMALLA, Nagaraju; DWIVEDI, Namrata; CHETLURU, Kiran Kumar; GADE, Srinivas Reddy; MUVVA, Venkateswarlu; SRIVASTAVA, Bindu
Patent: WO2011/25932 A2, 2011 ;
反应条件
1.1: 60 - 63 °C
2.1: ammonium acetate / methanol / 60 - 63 °C
3.1: sulfuric acid / methanol / -10 - 0 °C
3.2: 2 h / -10 - 0 °C
3.3: pH 8 - 9
4.1: isopropyl alcohol / 3 h / 25 - 30 °C
5.1: sodium carbonate / water / pH 8 - 9
6.1: water; lithium hydroxide hydrate / tetrahydrofuran / 0 - 30 °C
7.1: water; tetrahydrofuran / 6 h / 25 - 30 °C
7.2: pH 2
8.1: N-ethyl-N,N-diisopropylamine; 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; benzotriazol-1-ol / N,N-dimethyl-formamide / 13 h / 0 - 30 °C
9.1: hydrogenchloride / methanol / 12 h / 25 - 45 °C
View Scheme
参考文献
Mylan India Private Limited
Patent: US2012/108598 A1, 2012 ;