Hydrochloric Acid → HCID 73437352, compound

Temperature

27.5 °C

Into a dried 1 L 3 neck round bottom flask fitted with a nitrogen inlet, dropping funnel, thermometer, mechanical stirring and nitrogen outlet is added chloroform (300 ml) and 7-methylundecanol (93 g, 0.5 mol). Chlorosulfonic acid (60 g, 0.509 mol) is slowly added to the stirred mixture while maintaining 25-30° C. temperature with a ice bath. Once HCl evolution has stopped (1 hr.) slowly add sodium methoxide (25% in methanol) while keeping temperature at 25-30° C. until an aliquot at 5% concentration in water maintains a pH of 10.5. To the mixture is added hot ethanol (55° C., 2 L). The mixture is vacuum filtered immediately. The filtrate is concentrated to a slurry on a rotary evaporator, cooled and then poured into 2 L of ethyl ether. The mixture is chilled to 5° C., at which point crystallization occurs, and vacuum filtered. The crystals are dried in a vacuum oven at 50C for 3 hrs. to obtain a white solid.

1. customat 25-30° C.
2. concentrationat 5% concentration in water
3. additionTo the mixture is added hot ethanol (55° C., 2 L)
4. filtrationfiltered immediately
5. concentrationThe filtrate is concentrated to a slurry on a rotary evaporator
6. temperaturecooled
7. additionpoured into 2 L of ethyl ether
8. temperatureThe mixture is chilled to 5° C., at which point crystallization
9. filtrationvacuum filtered
10. dry with materialThe crystals are dried in a vacuum oven at 50C for 3 hrs
11. customto obtain a white solid

ORD record

ord-4e9b19511d364a689559889e829d4c71

Source dataset

uspto-grants-2002_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06335312B1