Synthetic Route of 22094-18-4,Some common heterocyclic compound, 22094-18-4, name is 1,3-Dibromo-2,2-dimethoxypropane, molecular formula is C5H10Br2O2, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
To a solution of 2-(2,5-difluoro-4-methylphenyl)acetonitrile (16.7 g, 100 mmol) in DMSO (200 mL) was added NaH (8 g, 200 mmol, 60% oil dispersion), portion-wise, at RT. The reaction was stirred for 1 h at RT, and then 1,3-dibromo-2,2-dimethoxypropane (39.3 g, 150 mmol) was added. The mixture was heated at 60 C for 6 h. The reaction was quenched with water (100 mL) at 0 C and extracted with EtOAc (2 x 100 mL). The organic extracts werecombined and washed with brine (2 x 50 mL), dried over Na2504, filtered, and concentrated under reduced pressure. The residue was purified by silica gel chromatography using petroleumn ether/EtOAc (4/1) as eluting solvents to afford the title compound as a yellow solid (12 g, 45% yield). ?H NMR(400 MHz, DMSO-d6)oe 7.36-7.28(m, 2H), 3.18(s, 3H), 3.05(s, 3H), 3.03 (d, J= 13.6 Hz, 2H), 2.77 (d, J= 13.6 Hz, 2H), 2.24 (d, J= 1.6 Hz, 3H). LCMS (ESI): mlz = 268.0[M+Hj.
The synthetic route of 22094-18-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; F. HOFFMANN-LA ROCHE AG; GENENTECH, INC.; RENE, Olivier; FAUBER, Benjamin; VESEY, David; WINSHIP, Paul; LADDUWAHETTY, Tammy; (97 pag.)WO2017/5668; (2017); A1;,
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