As a common heterocyclic compound, it belongs to quinuclidine compound,Quinuclidine-4-carboxylic acid hydrochloride,40117-63-3,Molecular formula: C8H14ClNO255,mainly used in chemical industry, its synthesis route is as follows.,3939-23-9
Tri-tert-butylphosphine (4.4 mL of a 1.0 M solution in toluene, 1.48 g, 0.05 mmol), palladium acetate (0.4 g,1.83 mmol) and sodium tert-butoxide (52.7 g, 549 mmol) were added to 2-6-a (20.423 g, 73.42 mmol) and 2-6-c(11.53 g, 73.42 mmol) a solution in degassed toluene (500 mL), and the mixture was warmed under reflux for 2 hr.The reaction mixture was cooled to room temperature, diluted with toluene and filtered over EtOAc. Dilute the filtrate with water and use aThe benzene was extracted and the organic phases were combined and evaporated under vacuum. The residue was passed through silica gel (heptane / dichloromethane)Filtration was carried out and crystallized from isopropanol. Obtaining 2-6-b 19.51 g, yield 75%; the resulting bromide 2-6-b(7.89 g, 20 mmol), pinacol borate (6.22 g, 24 mmol), 1,1′-bis(diphenylphosphino)-ferrocene-palladium dichloride(II) dichloromethane complex (0.49 g, 0.6 mmol), potassium acetate (5.90 g, 60 mmol) and 79 ml of toluene were reacted under refluxAfter 16 hours, cool, add 26 ml of water and stir for 30 minutes.The organic phase is separated and filtered through a short bed of diatomaceous earth, followed by organicThe solvent was distilled off and the crude product was recrystallized from heptane / toluene.The compound 2-6 was obtained in an amount of 6.58 g, yield 82%.
With the synthetic route has been constantly updated, we look forward to future research findings about 3-Bromo-10H-phenothiazine,belong thiazines compound
Reference£º
Patent; Changchun Hai Purunsi Technology Co., Ltd.; Zhang Hong; Cai Hui; (36 pag.)CN108530418; (2018); A;,
Thiazine – an overview | ScienceDirect Topics
Thiazine | C4H5NS – PubChem