5,7-Dimethyl-1,3-dibromoadamantane synthesis

Yield:21912-23-2 90%

Reaction Conditions:

with bromine;iron in 1,2-dichloro-ethane at 25;Temperature;Reagent/catalyst;Solvent;

Steps:

1.1-3.1 (1) Synthesis of 1,3-dibromo-5,7-dimethyladamantane

a) Add 108g (0.675mol) of bromine, 0.5g of iron powder, and 63g of 1,2-dichloroethane to a 250mL four-neck reaction bottle Stir well to get the reaction solution A; b) Heat the reaction liquid A to 25 to react; c) Slowly add 1,3-dimethyladamantane 50g (0.3mol) to the heated reaction solution A, and escape during the dropping Red-brown gas, absorbed with 5% sodium hydroxide solution, the reaction is monitored by gas chromatography, and cooled after completion of the reaction However, the reaction solution B was obtained at room temperature; d) Slowly add 320g of saturated sodium bisulfite solution to the reaction solution B until the red color in the reaction solution disappears completely, Separate liquid to get organic phase C and water phase D; e) The organic phase C is washed with 300g water, and the washed organic phase C is dried overnight with 20g anhydrous sodium sulfate; f) The organic phase C after drying spins out dichloroethane to obtain a crude product, which is rinsed with 25 g of cold cyclohexane to obtain 1,3-bis Bromo-5,7-dimethyladamantane, yield 90%, gas chromatography purity ≥99%;

References:

CN104592035,2016,B Location in patent:Paragraph 0031-0039; 0050-0058; 0069-0077