1,2-Hexadecanediol → Pentadecanediol Octadecanediol

Temperature

70 °C

Approximately 360 g of 1,2-mixed pentadecanediol to octadecanediol (commercially obtained as Vikol 158 from Viking Chemical Co. and containing about 28% 1,2-pentadecanediol, about 28% 1,2-hexadecanediol, about 28% 1,2-heptadecanediol and about 16% octadecanediol, all percentages by weight) were charged to a glass reactor equipped with heater, agitator, Dean-Stark tube with condenser and provision for blanketing the vapor space with nitrogen. The contents were heated to 70° C. to liquify the solids and 55 g of dimethyl phosphite were slowly added. The reaction mixture was heated to 110° C. and held for 2 hours, held at 120° C. for 1 hour and held at 130° C. for 1 hour. Methanol was observed forming and collecting in the trap. The crude product was vacuum stripped at 150° C. to remove volatile materials, producing 375 g of intermediate additive. The intermediate was an amber fluid which became waxy after cooling.

1. additionall percentages by weight) were charged to a glass reactor
2. customequipped with heater, agitator, Dean-Stark tube with condenser
3. additionwere slowly added
4. temperatureThe reaction mixture was heated to 110° C.
5. waitheld at 120° C. for 1 hour
6. waitheld at 130° C. for 1 hour
7. customcollecting in the trap
8. customstripped at 150° C.
9. customto remove volatile materials

ORD record

ord-47186f20d039468fbee398b1fe8e76a8

Source dataset

uspto-grants-1985_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04522629