Sodium Carbonate → HCID 54436504, compound

Participants

Reaction Steps

27.61 g (0.104 mol) (1a) was dissolved in 400 ml CH2Cl2. This solution was added dropwise to an ice-cooled solution of 36.03 g (0.208 mol) 3-chloroperbenzoic acid in 600 ml CH2Cl2 and 33.61 g (0.375 mol) NaHCO3 in 200 ml H2O. After the addition of (1a) the mixture was allowed to warm up to room temperature, and this was followed by another 2 hours' stirring. The reaction mixture was then poured into 500 ml 5% Na2CO3 solution. The organic layer was washed with 500 ml 5% Na2S2O3 solution. The CH2Cl2 was dried over MgSO4 and evaporated. The precipitate was purified by recrystallization from hexane/toluene. Yield: 26.65 g (91%); m.p.=170.3-170.9° C. (dec.)

Provenance & Evidence