cyclohexyl but-2-enoate

Conditions: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Cyclohexanol (220 g), crotonic acid (199 g), PTSA (8 g), and toluene (300 mL) were charged into a 2-L reaction flask fitted with a mechanical stirrer, a thermocouple, a Dean-Stark trap, and a condenser. The reaction mixture was heated to reflux at about 120-130° C. Water was removed azeotropically. The reaction was aged at reflux for about 4-5 hours until no more water evolved. The reaction mixture was cooled to room temperature and quenched with water (400 mL). The organic layer was separated and subsequently washed with sodium carbonate (5%, 300 mL), and further fractional distilled to provide but-2-enoic acid cyclohexyl ester (290 g) with a boiling point of 104° C. at 13 mmHg. fitted with a mechanical stirrer The reaction mixture was heated Water was removed azeotropically at reflux for about 4-5 hours until no more water The reaction mixture was cooled to room temperature quenched with water (400 mL) The organic layer was separated subsequently washed with sodium carbonate (5%, 300 mL) further fractional distilled

Conditions: temp:125.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: Cyclohexanol (220 g), crotonic acid (199 g), PTSA (8 g), and toluene (300 mL) were charged into a 2-L reaction flask fitted with a mechanical stirrer, a thermocouple, a Dean-Stark trap, and a condenser. The reaction mixture was heated to reflux at about 120-130° C. Water was removed azeotropically. The reaction was aged at reflux for about 4-5 hours until no more water evolved. The reaction mixture was cooled to room temperature and quenched with water (400 mL). The organic layer was separated and subsequently washed with sodium carbonate (5%, 300 mL), and further fractional distilled to provide but-2-enoic acid cyclohexyl ester (290 g) with a boiling point of 104° C. at 13 mmHg. fitted with a mechanical stirrer The reaction mixture was heated Water was removed azeotropically at reflux for about 4-5 hours until no more water The reaction mixture was cooled to room temperature quenched with water (400 mL) The organic layer was separated subsequently washed with sodium carbonate (5%, 300 mL) further fractional distilled