1,4-Dichlorobenzene → α-Methylstyrene dimer

Temperature

190 °C

Using the same procedure and equipment as in Example 1, the flask was charged with brominated styrene monomer (1004.2), dichlorobenzene (492 g), glycidyl methacrylate (5.11 g, 0.0359 mol), 2,4-diphenyl-4-methyl-1-pentene (20.13 g, 0.0851 mol) (α-methyl styrene dimer) and VAZO-52™ (1.03 g, 4.15 mmol). The solution was heated to about. 90° C. until exotherm. It then reached a peak temperature of 141° C. after which the mixture was heated to 190° C. over 5-10 min and held at 190° C. for 40-45 min. Heating was halted; the solution (1509.3 g) was transferred to a 2-liter bottle, and cooled to room temperature. The material was split into four parts. Each part was precipitated into a 5-liter flask of 3400 mL acetone and 400 mL methanol. The precipitate was filtered over frit, dried at ambient temperature for about 14 h and oven dried at 110° C. for 8 h. A white powder (881 g) was isolated.

1. temperatureThe solution was heated to about
2. custom90° C.
3. customa peak temperature of 141° C.
4. temperatureHeating
5. temperaturecooled to room temperature
6. customThe material was split into four parts
7. customEach part was precipitated into a 5-liter flask of 3400 mL acetone and 400 mL methanol
8. filtrationThe precipitate was filtered over frit
9. customdried at ambient temperature for about 14 h
10. customoven dried at 110° C. for 8 h

ORD record

ord-305fe872abfb4237b3d80c384e4db951

Source dataset

uspto-grants-2010_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07691947B2