SDS of cas: 2913-97-5, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 2913-97-5 as follows.
Compound 2: NaBH(OAc)3 (3,05 g ;14,4 mmol) was added to a solution of N- ethylaniline (1,16 g ; 9,6 mmol) and 2-phthalimidoacetaldehyde (1) (2,72 g, 14,4 mmol) in CH2C12 (28 mL). After 24 h at 20°C, CH2C12 was added and the organic phase was washed with H20, dried (MgS04) and evaporated. The crude product was purified by chromatography over silica gel (80:20 CH2Cl2-cyclohexane) to afford 2 as a yellow solid (2,71 g, 96 percent). 1H NMR (250 MHz, CDC13): delta 7,85 (m, 2H), 7,71 (m, 2H), 7.24 (t, J = 7,8 Hz, 2H), 6,86 (d, J = 7,8 Hz, 2H), 6.67 (t, J = 7,8 Hz, 1H), 3.91 (dd, J = 6,5, 8,1 Hz, 2H), 3,58 (dd, J = 6,5, 8,1 Hz, 2H), 3,46 (q, J = 6,9 Hz, 2H), 1.22 (t, J = 7,0 Hz, 3H). 13C NMR (63 MHz, CDC13): <5 168,0 (C), 147,2 (C), 133,7 (CH), 131 ,8 (C), 129,2 (CH), 123,0 (CH), 116,0 (CH), 111,9 (CH), 47,8 (CH2), 44,6 (CH2), 35,0 (CH2), 12,2 (CH3). MS: m/z = 295 (MH+). Anal, calcd for Ci8Hi8N202 (294,14), C 73.45, H 6,16, N 9,52. Found C 73,33, H 6,17, N 9,62.
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Reference:
Patent; UNIVERSITE PARIS DESCARTES; SLAMA-SCHWOK, Anny; BOUCHER, Jean-Luc; XU-LI, Yun; DEPREZ, Eric; HENRY, Etienne; DESSY, Chantal; FERON, Olivier; TARUS, Bogdan; WO2012/175516; (2012); A1;,
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