Synthetic Route of 107862-65-7, 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 107862-65-7 as follows.
The bicyclic compound 16 (9mmol, 973mg) was dissolved in dry CHCl3 (40mL) and NBS (10mmol, 1.73g) was added. The bright red reaction mixture was stirred for 5min at room temperature. The mixture was diluted in CHCl3 (20mL), washed with water (3×50mL), dried over MgSO4, and concentrated in vacuo. The crude brown solid was dissolved in Et2O and filtered through a thin layer of silica gel. Evaporation of the solvent afforded a light yellow crystalline product (1.43g) in 77% yield (MP 82.6-84.0C) from 14. It became dark after standing at room temperature and at a lower temperature. Mp: 82.6-84.0C; 1H NMR: delta=7.43 (s, 1H, CH), 4.16 (t, 3J=7.3, 2H, NCH2), 2.82-2.87 (m, 2H, =C-CH2), 2.58-2.66 (m, 2H, NCH2CH2); 13C NMR: delta=144.8 (C), 143.9 (CH), 86.7 (C-Br), 49.0 (CH2), 26.2 (CH2), 22.6 (CH2); GC-MS m/z (%): 188 (M++1, 64), 186 (63), 107 (93), 80 (49), 51 (100); FTIR (KCl): 2962, 2922, 2854, 1706, 1641, 1452, 1318, 1226, 1156, 1013, 986. HRMS m/z calcdfor C6H8N2Br: 186.9871. Found: 186.9873.
According to the analysis of related databases, 107862-65-7, the application of this compound in the production field has become more and more popular.
Reference:
Article; Galeta, Juraj; Tenora, Luka?; Man, Stanislav; Pota?ek, Milan; Tetrahedron; vol. 69; 34; (2013); p. 7139 – 7146;,
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