These common heterocyclic compound, 5414-19-7, name is 1-Bromo-2-(2-bromoethoxy)ethane, 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. COA of Formula: C4H8Br2O
Step a Intermediate 207 -Bromophenyl 2-ethyltetrahydro-2H-pyran-4-carboxylate A mixture of NaH (60% in mineral oil) (2.057 g, 51.4 mmol) in DMF (67 ml) stirred at 0 C was treated dropwise with a mixture of ethyl 2-(4-bromophenyl)acetate (5 g, 20.57 mmol) and 1 -bromo-2-(2-bromoethoxy)ethane (2.59 ml, 20.57 mmol) in 3 ml of diethyl ether. The mixture was allowed to warm to r.t. and stirred for 17 h. Mixture was quenched with water and sat. NH4CI. The mixture was extracted with EtOAc (x 3) and then organics washed with brine (x 3) and dried (MgS04), filtered and concentrated under reduced pressure. The residue was purified by column chromatography (Si02; 0 – 100 % EtOAc in petrol) to yield 4-bromophenyl 2-ethyltetrahydro-2H-pyran-4- carboxylate as a pale yellow oil (2.88 g, 45 %). ? NMR (400 MHz, CD2C12) 57.46 – 7.56 (m, 2H), 7.32 (m, 2H), 4.15 (m, 2H), 3.84 – 3.98 (m, 2H), 3.50 – 3.63 (m, 2H), 2.38 – 2.56 (m, 2H), 1.95 (m, 2H), 1.21 (m, 3H)
The synthetic route of 1-Bromo-2-(2-bromoethoxy)ethane has been constantly updated, and we look forward to future research findings.
Reference:
Patent; TAKEDA PHARMACEUTICAL COMPANY LIMITED; RUPRAH, Parminder, Kaur; MERCHANT, Kevin, John; WALSH, Louise, Marie; KERR, Catrina, Morven; FIELDHOUSE, Charlotte; HARRISSON, David; MAINE, Stephanie; HAZEL, Katherine; WO2013/27001; (2013); A1;,
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