Reference of 135450-23-6 , The common heterocyclic compound, 135450-23-6, name is 6-(Chloromethyl)-2-cyanopyridine, molecular formula is C7H5ClN2, 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.
A solution of 1-(1-methyl-1 /-/-tetrazol-5-yl)-1,3-dihydro-2H-benzo[d]imidazole-2-thione H (26 mg, 0.1 1 mmol) in dry DMF (1 mL) was treated with a solution of A/-(6-(bromomethyl)pyridin- 2-yl)-2,2-difluoro-2-phenoxyacetamide E (49 mg, 0.14 mmol) in dry THF (0.7 mL) and caesium carbonate (60 mg, 0.18 mmol) was added. The mixture was stirred at RT for 100 min then diluted with EtOAc (20 mL), washed with water (3 x 20 mL) and brine, dried (MgSCU) and chromatographed on silica (4 g Puriflash cartridge) eluting with 0-50% EtOAc / PE to give 2,2-difluoro-/V-(6-(((1-(1-methyl-1H-tetrazol-5-yl)-1H-benzo[d]imidazol-2- yl)thio)methyl)pyridin-2-yl)-2-phenoxyacetamide 1 (48 mg, 84%) as a colourless gum. 1H N MR (500 MHz, CDC) delta 8.90 (s, 1H), 8.13 (d, J = 8.3 Hz, 1H), 7.77 (d, J = 8.0 Hz, 1H), 7.74 – 7.68 (m, 1H), 7.45 – 7.33 (m, 3H), 7.32 – 7.26 (m, 5H), 7.07 – 7.00 (m, 1H), 4.67 (s, 2H), 3.92 (s, 3H); LCMS (method B): 3.28 min (509, MH+). Potassium carbonate was used instead of caesium carbonate
The synthetic route of 135450-23-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; REDAG CROP PROTECTION LTD; URCH, Christopher, John; BUTLIN, Roger, John; CHRISTOU, Stephania; BOOTH, Rebecca, Kathryn; (111 pag.)WO2018/130838; (2018); A1;,
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