Butanal → HCID 12476960, Verbindung

Temperatur

-30 °C

56 mmol of n-butyllithium (35 ml of a 1.6 M solution in hexane) were added with stirring to a solution of 2-methyl-1,3-dithian (7 g, 52.1 mmol) in 100 ml of dry tetrahydrofuran at −30° C. under argon. After stirring at −30° C. for 2 hours, the mixture was cooled to −78° C. 4.2 g (58.3 mmol) of freshly distilled n-butyraldehyde were added dropwise in the course of 15 minutes and the mixture was stirred for a further 30 minutes. After warming to 20° C., it was poured into a beaker containing 300 ml of water and 100 ml of n-hexane. The organic phase was separated off and the aqueous phase was extracted three times with 50 ml of dichloromethane in each case. The combined organic phases were washed with 10% strength by weight potassium hydroxide solution, water and concentrated sodium chloride solution, dried over anhydrous sodium sulfate and then distilled. 8.82 g of 2-(1-hydroxybutyl)-2-methyl-1,3-dithian were isolated as a colorless oil.

1. temperaturethe mixture was cooled to −78° C
2. stirringthe mixture was stirred for a further 30 minutes
3. temperatureAfter warming to 20° C.
4. additionit was poured into a beaker
5. customThe organic phase was separated off
6. extractionthe aqueous phase was extracted three times with 50 ml of dichloromethane in each case
7. washThe combined organic phases were washed with 10% strength by weight potassium hydroxide solution, water and concentrated sodium chloride solution
8. dry with materialdried over anhydrous sodium sulfate
9. distillationdistilled

ORD-Eintrag

ord-4a3edc1b5e0642e8be21e20e3154a1ca

Quelldatensatz

uspto-grants-2001_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06245328B1