Reference of 33252-28-7, With the rapid development and complex challenges of chemical substances, the synthesis of new drugs is usually one of the most effective ways to increase yield.33252-28-7, name is 6-Chloronicotinonitrile, molecular formula is C6H3ClN2, molecular weight is 138.55, as common compound, the synthetic route is as follows.
[N- (5-CYANO-2-PHENYL-LH-PYRROLOF2, 3-BLPYRIDIN-3-YL)-ACETAMIDE] [6-CHLORO-NICOTINONITRILE] (1.38 g, 10 mmol) was dissolved in 1,4-dioxane (50 ml). Hydrazine hydrate (0.525 ml, 10.4 mmol) was added and the resulting solution stirred for 1.5h, whereupon it was concentrated in vacuo. The residue was chromatographed (silica gel, gradient ethyl acetate/heptane from 1: 1 to 1: 0). The slower running component was concentrated in vacuo to afford the 6-hydrazino-nicotinonitrile monohydrate [0.80 g, 53%, APCI-MS m/z: 135.2 [MH+] ]. Part of this hydrazine (67 mg, 0.5 mmol) and [N- (2-OXO-2-] [PHENYL-ETHYL)-ACETAMIDE] (85 mg, 0.5 mmol) were fused together for lh at 230 [C.] The reaction mixture was allowed to cool and the glassy solid suspended in warm dichloromethane/methanol (7: 3 mixture) and then filtered. The solid was further washed with hot [ACETONITRILE/N,] [N-DIMETHYLFORMAMIDE] (9: 1 mixture) and finally acetonitrile. This afforded the title compound as a grey powder (25 mg, 18%). ‘H-NMR (DMSO-d6) : [B] 12.64 [(1H,] s); 9.66 [(1H,] s); 8.62 [(1H,] s); 8.27 (1H, s); 7.84 (2H, d); 7.52 (2H, t); 7.42 [(1H,] t); 2.10 (3H, s). [‘3C-NMR] (DMSO-d6) : [8] 147.3 ; 145.8 ; 134.0 ; 131.5 ; 129.9 ; 128.8 ; 128.7 ; 127.5 ; 118.8 ; 117.6 ; 110.1 ; 99.9 ; [22. 7.] APCI-MS m/z : 277.1 [[MH+].]
The chemical industry reduces the impact on the environment during synthesis 33252-28-7, I believe this compound will play a more active role in future production and life.
Reference:
Patent; ASTRAZENECA AB; WO2004/16609; (2004); A1;,
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