Sodium Hydroxide → HCID 19790452, compound

Participants

Reaction Conditions

Reaction Steps

Into a reactor as described in Example 1 and with similar procedure there were charged 40.9 kg of water and, with agitation, 24.5 kg of sodium 4-phenolsulfonate. After an additional 10 minutes of agitation, there was added 9.7 kg of 50%, by weight, sodium hydroxide over a period of 15 minutes. There were then added 9.72 g of product and 68.1 kg of methylethyl ketone. After heating the mixture to 50° C. there was added 19.5 kg of n-hexylchloroformate over a period of 15 minutes. During addition of the chloroformate the batch temperature increased to about 65° C. and the reaction allowed to proceed with agitation for a period of 30 minutes at a temperature in the range of 65° C.-70° C. After completion of the reaction the mixture was cooled to below 50° C. and allowed to settle into two phases. The top organic layer containing n-hexylsulfophenyl carbonate was separated from the bottom saturated layer, and was washed with 22.72 kg of a 33 percent aqueous solution of sodium sulfate. After thorough mixing the mixture was allowed to settle. The top organic layer was separated from the bottom salt layer and the procedure with sodium sulfate repeated two more times. The organic layer was pan dried with vacuum. About 45.4 kg of n-hexyl sulfophenyl carbonate was obtained which contained 0.92 percent di-n-hexyl carbonate as indicated by analysis (gc) of a cyclohexane extract.

Provenance & Evidence