Propanal → HCID 23342697, compound

Temperature

10 °C

Propanal (81 mL, 1.11 mol) and allyl alcohol (100 g, 1.72 mol) were dissolved in hexane (400 mL) under a nitrogen atmosphere. To the solution, magnesium sulfate (82.90 g, 0.69 mol) was added, and the mixture was stirred. This mixture was cooled to 10° C. or lower, and p-toluenesulfonic acid monohydrate (3.28 g, 0.017 mol) was added thereto. The reaction mixture was stirred at 15° C. or lower for 1 hour. To the reaction mixture, potassium carbonate (2.38 g) and water (400 mL) were added in this order. The mixture was stirred until insoluble matter was dissolved. An organic layer was separated and then washed with water (100 mL). The obtained organic layer was concentrated under reduced pressure, and the residue was distilled (approximately 25 mmHg, 67-72° C.) to obtain the title compound (113.67 g, yield: 85%, colorless oil substance).

1. stirringThe reaction mixture was stirred at 15° C. or lower for 1 hour
2. stirringThe mixture was stirred until insoluble matter
3. dissolutionwas dissolved
4. customAn organic layer was separated
5. washwashed with water (100 mL)
6. concentrationThe obtained organic layer was concentrated under reduced pressure
7. distillationthe residue was distilled (approximately 25 mmHg, 67-72° C.)

ORD record

ord-368ed6e411de418c88dfa9155f7e098e

Source dataset

uspto-grants-2015_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09162971B2