Reaction #2018771
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07847126B2
Conditions: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: In a round-bottomed flask, 60.6 mg of copper(I) bromide-dimethyl sulphide complex and 51.2 mg of lithium bromide are initially charged under protective gas. 20 ml of hexane, 4 ml of dichlorophenylphosphine and another 19 ml of hexane are subsequently added. The reaction solution is cooled to 0° C. 32.4 ml of a 2 M solution of tert-butylmagnesium chloride in ether are then slowly added dropwise. The mixture is subsequently allowed to slowly adjust to room temperature and is then stirred at room temperature for a further two hours. For workup, the mixture is cautiously admixed with 75 ml of degassed 2 M HBF4. Another 5 ml of 8 M HBF4 are then additionally added and stirred for 15 min. Filtration with suction is then effected and the filter cake is washed with a little cold water. The residue is dried under reduced pressure to constant weight. Yield: 7.9 g (86% of theory) purity >99%. to slowly adjust to room temperature stirred for 15 min Filtration with suction the filter cake is washed with a little cold water The residue is dried under reduced pressure to constant weight
Source ID: ord-e89df2b5f1c3483bbef092f5942427d3