Nitrogen → Allyl acetoacetate

In a 2 l flask equipped with a magnetic stirrer, equipped for a Vigreaux column for distillation, a heating mantle and N2, there was added 4.0 mole (432 ml) of methyl acetoacetate and 8.0 mole (464.6 g) of allyl alcohol. The reaction mixture was distilled for 12 hours at 92° C. There was added 136 ml (2.0 mole) of allyl alcohol and the mixture was distilled 23 hours. There was then added 136 ml (2.0 mole) of allyl alcohol and the mixture was distilled 16 hours. The reaction mixture was then distilled under vacuum and product was collected at 105°-110° C./35 mm Hg. There was obtained 414 g of allyl acetoacetate (73% yield). ##STR221##

1. customIn a 2 l flask equipped with a magnetic stirrer
2. customequipped for a Vigreaux column for distillation
3. distillationThe reaction mixture was distilled for 12 hours at 92° C
4. distillationthe mixture was distilled 23 hours
5. distillationthe mixture was distilled 16 hours
6. distillationThe reaction mixture was then distilled under vacuum and product
7. customwas collected at 105°-110° C./35 mm Hg

ORDレコード

ord-9b317240b3134c958df20010ade00b41

出典データセット

uspto-grants-1987_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04644061