تفاعل #2499

معادلة التفاعل

octanal

benzaldehyde

pyrrolidine

diphenylamine

acetic acid

NaOH

acetic acid

octanal

→

α-hexylcinnamaldehyde

ظروف التفاعل

المعالجة

1. 1
   أخرىThe reaction was carried out in a 2.5 litre double-walled glass reactor
2. 2
   أخرىprovided with a cooler, turbine stirrer (6 blades)
3. 3
   أخرىwere metered in at 85° C
4. 4
   workup.WAITto continue at 85° C. for a further 15 minutes
5. 5
   درجة الحرارةThe reaction mixture was cooled to 65° C.
6. 6
   أخرىthe reaction mixture was separated at 50° C., over a period of 5 to 6 minutes

الإجراء التجريبي

The reaction was carried out in a 2.5 litre double-walled glass reactor provided with a cooler, turbine stirrer (6 blades), thermocouple and a submerged metering tube. A mixture of 1065 grams of benzaldehyde (10.0 mol), 48.8 grams of pyrrolidine (0.679 mol) and 1.8 grams of diphenylamine was heated to 85° C. Over a period of 180 minutes, 878 grams of acidified (0.34 meq/gram) octanal (6.648 mol) were metered in at 85° C. Acidification of the octanal was effected with 16.9 grams of acetic acid (0.281 mol). The reaction was allowed to continue at 85° C. for a further 15 minutes. The reaction mixture was cooled to 65° C. and washed at 50° C., for 15 minutes, with 500.3 grams of 5% strength aqueous NaOH solution (0.625 mol). After neutralization with 78 grams of acetic acid (1.30 mol) for 15 minutes at 50° C., the reaction mixture was separated at 50° C., over a period of 5 to 6 minutes. The organic layer (1869.8 grams) contained 25.5% of benzaldehyde, 2.1% of octanal, 59.8% of α-hexylcinnamaldehyde and 4.6% of α-hexyldecenal. The degrees of conversion of benzaldehyde and octanal were 55.2% and 95.5%, respectively. The selectivity in producing α-hexylcinnamaldehyde was 93.5% with respect to benzaldehyde and 81.4% with respect to octanal.

المصدر