Extracurricular laboratory: Synthetic route of 22094-18-4

The synthetic route of 22094-18-4 has been constantly updated, and we look forward to future research findings.

Reference of 22094-18-4, These common heterocyclic compound, 22094-18-4, name is 1,3-Dibromo-2,2-dimethoxypropane, its 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.

1 -(3 ,4-dichlorophenyl)-3 ,3 -dimethoxycyclobutanecarboxamide[1 182] 3,4-Dichlorophenylacetonitrile (9.30 g, 50 mmol), l,3-dibromo-2,2- dimethoxypropane (13.10 g, 50 mmol), and sodium tert-butoxide (10.57 g, 110 mmol) in DMSO (100 mL) and water (5 mL) were heated at 125C for 1 hour, then stirred at ambient temperature for 20 hours. The reaction mixture was diluted with water and extracted three times with diethyl ether. The organic layers were combined, washed with brine, dried with MgS04, filtered, and concentrated. The crude product was triturated with 1 : 1 diethyl ether / hexanes, and the solid collected by filtration was Example 82A (7.16 g, 23.54 mmol, 47.1% yield). XH NMR (300 MHz, DMSO-d6) ? 7.61 – 7.55 (m, 2H), 7.37 (s, 1H), 7.29 (dd, J= 8.4, 2.2 Hz, 1H), 6.95 (s, 1H), 3.05 (s, 3H), 2.99 (s, 3H), 2.97 – 2.89 (m, 2H), 2.46 – 2.37 (m, 2H).

The synthetic route of 22094-18-4 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; ABBVIE INC.; BAYBURT, Erol K.; CLAPHAM, Bruce; COX, Phil B.; DAANEN, Jerome F.; GOMTSYAN, Arthur; KORT, Michael E.; KYM, Philip R.; VOIGHT, Eric A.; SCHMIDT, Robert G.; DART, Michael J.; GFESSER, Gregory; WO2013/62964; (2013); A2;,
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