Hydrochloric Acid → HCID 55302371, compound

Temperature

100 °C

To a stirred solution of 20% HCl (7 ml) was added bis(1-methylethyl) 3,3-dimethoxycyclobutane-1,1-dicarboxylate (2.5 g, 8.7 mmol) at RT. The resulting mixture was heated at 100° C. overnight and then cooled to RT and extracted with diethyl ether (3×20 ml). The organic phases were combined, dried (Na2SO4), filtered and concentrated at reduced pressure. The resulting light brown oil was slurried in DCM (2 ml) and the resulting solid collected by filtration, washed with pentane and dried at reduced pressure to yield a pale brown solid (530 mg, 47%).

1. temperaturecooled to RT
2. extractionextracted with diethyl ether (3×20 ml)
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. concentrationconcentrated at reduced pressure
6. filtrationthe resulting solid collected by filtration
7. washwashed with pentane
8. customdried at reduced pressure

ORD record

ord-0b747cd768f040dc984050640f24afc9

Source dataset

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08691804B2