Sodium Hydroxide → HCID 15545532, compound

Participants

Reaction Conditions

Reaction Steps

20.05 kg (26.7 mol) of methyl 3-(4-cyano-phenoxymethyl)-benzoate are dissolved in 100 litres of THF and 40 litres of methanol. At 40 to 45° C., 8.51 kg of sodium boranate are added in batches. The reaction is completed by stirring the reaction mixture at 61 to 63° C. for about 5 hours. The reaction mixture is then cooled to 25° C. and 90 litres of a 15% sodium hydroxide solution are added. After stirring, the aqueous supernatant is separated off and mixed with 30 litres of a 22.5% sodium hydroxide solution. After stirring, the aqueous supernatant is separated off and from this about 100 litres of solvent are distilled off at a sump temperature of 63 to 75° C. The distillation residue is crystallised by the addition of 20 litres of isopropanol at 50 to 60° C. and 150 litres of water at 40 to 50° C. After the suspension has been cooled to 20 to 30° C. the crystals are separated off, washed with 60 to 100 litres of water and batchwise with 25 litres of cold isopropanol and dried in vacuo.

Provenance & Evidence