Methanol → HCID 178443269, compound

Temperature

30 °C

The 0.5 liter reactor was charged with 1,2-dichloroethane, 200 mL, methanol, 20 mL, 1-octene, 50 mL, and Ex. 1, 100 mg (0.13 mmole). The vessel was assembled and pressure tested then charged as follows: enough propylene was added to give a pressure of 124 psig at 18° C. Carbon monoxide was added to give and maintain a pressure of approximately 1000 psig. Carbon monoxide was made-up during the course of the run by a demand feed regulator. Contents were heated to a setpoint of 30° C. and stirred at 1250 rpm for a total of 21 hours and 35 minutes. The product appeared soluble in the reaction solvent. All volatiles were evaporated under nitrogen streaming at room temperature in order to determine if a product had been obtained. The remaining residue was redissolved in 1,2-dichloroethane, 200 mL, then treated with 3 g of activated alumina. The mixture was filtered and solvent was evaporated by nitrogen streaming. The polymer sheet was further dried under vacuum at 60° C. for 24 hours. A total of 10.910 g of polymer was recovered.

1. additionpressure tested then charged
2. customto give a pressure of 124 psig at 18° C
3. customto give
4. temperaturemaintain a pressure of approximately 1000 psig
5. customAll volatiles were evaporated under nitrogen streaming at room temperature in order
6. customhad been obtained
7. addition200 mL, then treated with 3 g of activated alumina
8. filtrationThe mixture was filtered
9. customsolvent was evaporated by nitrogen streaming
10. customThe polymer sheet was further dried under vacuum at 60° C. for 24 hours
11. customA total of 10.910 g of polymer was recovered

ORD record

ord-712843a410524a5dba54a1110a1b9547

Source dataset

uspto-grants-2001_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06239250B1