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. 17570-98-8, name is 2-(Bromoacetyl)pyridine hydrobromide, molecular formula is C7H7Br2NO, 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. name: 2-(Bromoacetyl)pyridine hydrobromide
[0284] 7V-(3-Methylphenyl)-4-(2-pyridinyl)-l,3-thiazol-2-amine (68). A mixture of bromoketone hydrobromide 67 (0.96 g, 3.4 mmol) and 3- methylphenylthiourea (4) (0.57 g, 3.4 mmol) in EtOH (25 mL) was stirred at reflux temperature for 3 h. The mixture was cooled to 20 0C, diluted with water (40 mL), the pH adjusted to ca. 8 with aqueous NH3 and the mixture stirred at 0 0C for 1 h. The precipitate was filtered, washed with water (5 mL) and dried. The crude solid was purified by column chromatography, eluting with EtOAc, to give amine 68 (0.74 g, 81%) as a cream powder: mp (EtOAc) 164-166 0C; 1H NMR delta 10.20 (br s, 1 H, NH), 8.58 (ddd, J= 4.7, 1.7, 0.8 Hz, 1 H, H-6′), 7.99 (dt, J= 7.9, 0.9 Hz, 1 H, H-3′), 7.99 (ddd, J= 7.9, 7.5, 1.8 Hz, 1 H, H-4′), 7.58 (br d, J= 8.1 Hz, 1 H, H- 6′), 7.52 (s, 1 H, H-5), 7.47 (br s, 1 H, H-2″), 7.31 (ddd, J= 7.5, 4.7, 1.2 Hz, 1 H, H-5′), 7.24 (t, J= 7.8 Hz, 1 H, H-5″), 6.80 (br d, J= 7.5 Hz, 1 H, H-4″), 2.33 (s, 3
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Reference:
Patent; THE BOARD OF TRUSTEES OF THE LELAND STANFORD JUNIOR UNIVERSITY; AUCKLAND UNISERVICES LIMITED; WO2009/114552; (2009); A1;,
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