Hydrochloric Acid → 2-(Methacryloyloxy)ethyl 2-acetylpent-2-enoate

Temperatur

0 °C

To a magnetically stirred, 1000 mL, round bottom flask were added 200 mL of propionaldehyde and 587 mL 2-(methacryloyloxy)ethyl 3-oxobutanoate. The reaction mixture was cooled to 0° C., in an ice bath, and then 3 to 5 mL of piperidine was added dropwise over one minute. The mixture was stirred at 0° C., for 2 hours, and then allowed to warm to room temperature over the course of 2-2.5 hours. To the reaction mixture was slowly added 30 mL of 3N HCl, over about one minute, to neutralize the piperdine. The mixture was poured into a separatory funnel, and then 150 mL of deionized water was added. The mixture was shaken, and then the aqueous layer was separated and disposed of. The reaction mixture was washed three more times with 150 mL of deionized water, each time, and then dried over MgSO4. The reaction mixture was filtered, and then stabilized with 10 mass ppm of 4-hydroxy-TEMPO. The dried reaction mixture was used without further purification.

1. stirringThe mixture was stirred at 0° C., for 2 hours
2. temperatureto warm to room temperature over the course of 2-2.5 hours
3. additionThe mixture was poured into a separatory funnel
4. stirringThe mixture was shaken
5. customthe aqueous layer was separated
6. washThe reaction mixture was washed three more times with 150 mL of deionized water
7. dry with materialeach time, and then dried over MgSO4
8. filtrationThe reaction mixture was filtered
9. customThe dried reaction mixture
10. customwas used without further purification

ORD-Eintrag

ord-ba80ac078bba4eb4a68df90d8be0075a

Quelldatensatz

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09388260B2