2-(4-BroMo-phenyl)-3-Methyl-butyronitrile synthesis
- Product Name:2-(4-BroMo-phenyl)-3-Methyl-butyronitrile
- CAS Number:51632-12-3
- Molecular formula:C11H12BrN
- Molecular Weight:238.12
Yield:-
Reaction Conditions:
Stage #1: 4-Bromophenylacetonitrilewith sodium hydride in N,N-dimethyl-formamide;mineral oil; for 0.25 h;
Stage #2: isopropyl bromide in N,N-dimethyl-formamide;mineral oil at 20; for 2 h;
Steps:
To a solution of R-1 (20.0 g, 0.102 mol) in DMF (300 mL) at 0 °C is added NaH (60% in oil suspension, 4.28 g, 0.107 mol) slowly. The mixture is then stirred for a further 15 minutes and 2-bromopropane (9.60 mL, 0.107 mol) is added. The reaction mixture is allowed to warm to room temperature, stirring continued for 2 hours and then concentrated in vacuo. The residue is partitioned between CH2CI2 and brine. The combined organics are dried with Na2S04, filtered and concentrated in vacuo. The residue is purified by flash chromatography (Si02, 0-15% EtOAc in heptane) to give 1-1 (21.3 g); m/z 238.3, 240.2 [M/M+2H]
References:
WO2012/24150,2012,A1 Location in patent:Page/Page column 109
