33348-34-4, name is 4-Amino-3-iodobenzonitrile, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. name: 4-Amino-3-iodobenzonitrile
Preparation 52; 6-Cyano-2,3,4,9-tetrahydro-lH-carbazol-3-yl)-carbamic acid tert-butyl esterAs described in C Chen et al, J. Org. Chem. (1997) 62, 2676-2677, mix 3- iodo-4-aminobenzonitrile (T. H. Jonckers, et al, J. Med. Chem. 45 (16) 3497-3508 (2002)) (1.3 g, 5.3 mmol) and (4-oxo-cyclohexyl)-carbamic acid tert-butyl ester (3.4 g, 16 mmol) l,4-diazobicyclo[2.2.2]octane (DABCO)(1.8 g, 16 mmol), magnesium sulfate (960 mg, 8 mmol) and DMF (30 mL). Sparge the stirred mixture with nitrogen for 10 min and add palladium(II) acetate (58 mg, 0.26 mmol) and place in a 105 C pre-heated oil bath. After 18 h, cool and dilute with EtOAc. Gravity filter the reaction into a separatory funnel and shake with water/EtOAc. Dry the organic layer (MgSO4) and concentrate to give a dark brown oil. Triturate with hexane (insoluble material is starting ketone). Concentrate the hexane solution and purify by silica gel chromatography (120 g), eluting with methylene chloride (0-40 min), then 10% EtOAc/methylene chloride (40-70 min) to give 550 mg (33%) of an off- white foam. MS (ES): m/z 312 (M+l), 310 (M-I); HPLC: R1 = 2.30 min, (97%).
The synthetic route of 33348-34-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ELI LILLY AND COMPANY; WO2007/2181; (2007); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com