Reference of 62226-17-9 , The common heterocyclic compound, 62226-17-9, name is 4-Chlorothieno[2,3-b]pyridine, molecular formula is C7H4ClNS, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
To a solution of 4-chlorothieno[2,3- Z>]pyridine (450 mg, 2.65 mmol, 1 eq.) in DCM (14.7 mL) was added 3-chloroperoxybenzoic acid (1.78 g, 7.95 mmol, 3 eq.) over 15 minutes. After three hours, the reaction was quenched with 10% NaS2C>3 solution and washed with 10% K2CO3. The aqueous layer was back extracted with 3: 1 CHCI3/IPA solution. The organic layers were combined, dried (MgS04), filtered and concentrated in vacuo. Purification by flash chromatography on silica gel afforded 500 mg (99%) of the title compound. XH NMR (400 MHz, DMSO-c) delta 8.42 (d, J = 6.6 Hz, 1H), 8.06 (d, J = 5.7 Hz, 1H), 7.65 (d, J = 6.6 Hz, 1H), 7.54 (d, J= 5.7 Hz, 1H); ES- MS [M+l]+: 186.4.
The synthetic route of 62226-17-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; VANDERBILT UNIVERSITY; LINDSLEY, Craig W.; CONN, P., Jeffrey; BOLLINGER, Katrina A.; ENGERS, Darren W.; BLOBAUM, Anna L.; ENGERS, Julie L.; ROOK, Jerri M.; (96 pag.)WO2018/63552; (2018); A1;,
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