As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 89510-90-7, name is 2-Chloro-5-fluoro-4-pyridinamine, molecular formula is C5H4ClFN2, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. Formula: C5H4ClFN2
2-(5-chloro-2-methoxy-phenyl)acetic acid (753 mg, 3.75 mmol) in thionyl 1 mL, 68.24 mmol) was stirred at 70 C for 1 hour. The resulting mixture was to dryness and azeotroped with toluene (2 x 10 mL). The crude residue was DMF (10 mL) and treated dropwise with a solution of 2-chloro-5-fluoro-pyridin- 0 mg, 3.41 mmol) in DMF (3 mL) followed by DIPEA (1.49 mL, 8.53 mmol). at room temperature under an inert atmosphere for 16 hours, the mixture was tOAc (100 mL) and washed with water (2 x 50 mL) and brine (2 x50 mL). The on was dried over Na2SO4 and concentrated in vacuo. The crude material was 18 reverse phase chromatography eluting with 0-100% MeCN in water with acid modifier to afford the titled compound as a light yellow solid. 0 MHz, DMSO-d6) delta 10.58 (s, 1H), 8.41 (d, J = 2.7 Hz, 1H), 8.24 (d, J = 5.6 3-7.28 (m, 2H), 7.01 (d, J = 9.5 Hz, 1H), 3.83 (s, 2H), 3.75 (s, 3H). hod E): Rt 1.25 mins; MS m/z 328.9, 330.9= [M+H]+
With the rapid development of chemical substances, we look forward to future research findings about 89510-90-7.
Reference:
Patent; ENTERPRISE THERAPEUTICS LIMITED; COLLINGWOOD, Stephen; MCCARTHY, Clive; HARGRAVE, Jonathan, David; HAY, Duncan, Alexander; SCHOFIELD, Thomas, Beauregard; ELLAM, Sarah; BUXTON, Craig; HABGOOD, Matthew; INGRAM, Peter; MA, Chun Yan; NAPIER, Spencer; SHAIKH, Abdul; SMITH, Matthew; STIMSON, Christopher; WALKER, Edward; (401 pag.)WO2019/145726; (2019); A1;,
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