tert-Butyl acrylate → Hydroxystyrene

Temperatur

60 °C

A 22 L reactor was charged with 2.919 kg acetoxystyrene, 1.538 kg t-butyl acrylate, 231 g BPO and 6 L toluene. The reactor was purged with nitrogen, and the reaction solution was heated at 60° C. under a N2 atmosphere for 23 h. The solution was then cooled to room temperature, diluted with an additional 12 L of toluene, and 248 L of heptane:isopropyl alcohol (30:1) was added. The precipitate was collected by vacuum filtration, and washed with 24 L heptane. The solid was recrystalized by first dissolving it in 15 L acetone and then adding 300 L isopropyl alcohol:water (51:24 v/v). The product was collected by vacuum filtration, rinsed with 30 L 1:1 isoproyl alcohol:water, and then dried at 50-55° C. under vacuum to a constant weight.

1. customThe reactor was purged with nitrogen
2. temperatureThe solution was then cooled to room temperature
3. additiondiluted with an additional 12 L of toluene, and 248 L of heptane:isopropyl alcohol (30:1)
4. additionwas added
5. filtrationThe precipitate was collected by vacuum filtration
6. washwashed with 24 L heptane
7. customThe solid was recrystalized
8. dissolutionby first dissolving it in 15 L acetone
9. additionadding 300 L isopropyl alcohol:water (51:24 v/v)
10. filtrationThe product was collected by vacuum filtration
11. washrinsed with 30 L 1:1 isoproyl alcohol
12. dry with materialwater, and then dried at 50-55° C. under vacuum to a constant weight

ORD-Eintrag

ord-4990dfe89939464a9a677cbd8c4759f1

Quelldatensatz

uspto-grants-2002_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06365321B1