Water → Crotonaldehyde dicrotyl acetal

Temperature

70 °C

In a 300-ml three-necked flask equipped with a water separator, 70 g (1 mole) of crotonaldehyde, 144 g (2 mole) of crotyl alcohol, 3 mg of stannous chloride dihydrate and 40 g of hexane were charged. The resulting mixture was heated at 70° C. under atmospheric pressure and for 4 hours in a nitrogen atmosphere while removing the water formed from the reaction mixture by azeotropic distillation. When water was no longer distilled, the solvent (hexane) and unreacted starting materials were distilled off under reduced pressure. Distillation of the residue under reduced pressure gave 182.2 g of crotonaldehyde dicrotyl acetal [R1 =a 1-propenyl group, R2 =a hydrogen atom and R3 =a crotyl group) (boiling point: 120° C./25 mmHg) (yield: 91.9%).

1. additionwere charged
2. customwhile removing the water
3. customformed from the reaction mixture by azeotropic distillation
4. distillationWhen water was no longer distilled
5. distillationwere distilled off under reduced pressure
6. distillationDistillation of the residue under reduced pressure

ORD record

ord-c6b5141dbf474f59955fa7ea33578389

Source dataset

uspto-grants-1998_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05792876