Related Products of 139512-70-2, 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. 139512-70-2 name is 4-Chloro-5-fluorobenzene-1,2-diamine, This 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.
4-Chloro-5-fluoro-benzene-1,2-diamine (5.20 g; 32.4 mmoles) and 3,3,3-trifluoro-2-hydroxy-propionic acid (7.00 g; 48.6 mmoles) were suspended in 6N HCl (9 mL; 54 mmoles) under a nitrogen atmosphere. The reaction was stirred vigorously and heated to 108C for 18 hrs, then cooled to room temperature. The reaction was diluted with water (100 mL) and with ethyl acetate (100 mL), then sodium bicarbonate (6.90 g; 81.00 mmoles) was added slowly and in portions to quench the reaction. The aqueous layer was separated and extracted with ethyl acetate (3×40 mL). The extracts were combined, washed with water (30 mL) and brine (30 mL), then dried over Na2SO4. The filtrate was concentrated in vacuo to yield a crude brown solid which was then purified by column chromatography (SiO2; 30% ethyl acetate/CH2Cl2) to yield the title compound as an off-white solid. 1H NMR (400 MHz, CD3CN) delta 7.74 (d, J = 6.7 Hz, 1 H), delta 7.49 (d, J =9.5,1 H), delta 5.41 (q, J = 6.8 Hz, 1 H), delta 5.16 (br s, 1 H), delta 2.35 (s, 6H) MS calculated for C9H5ClF4N2O: 268.00 MS measured: 269 (M+H); 267 (M-H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 4-Chloro-5-fluorobenzene-1,2-diamine, and friends who are interested can also refer to it.
Reference:
Patent; JANSSEN PHARMACEUTICA N.V.; WO2006/39243; (2006); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics