Tetrahydrofuran → HCID 54454059, compound

Temperature

0 °C

A solution of 3-butene-2-ol (8.7 mL, 100 mmol) in THF (50 mL) was added to potassium hydride (KH, 600 mg, 15 mmol) over 15 min. The resulting alkoxide solution was added to a stirred solution of trichloroacetonitrile (10.03 mL, 100 mmol) in ether (100 mL) at -10° C. The solution was stirred at 0° C. for 3 h, followed by removal of solvent under reduced pressure (temperature <25° C.); pentane (400 mL) and methanol (1 mL) were added, and the mixture filtered. Concentration afforded a yellow oil (17.4 g). The oil was dissolved in xylene (450 mL) and refluxed for 2.5 h. The solvent was removed to yield 16.8 g of the title compound as a white solid.

1. customfollowed by removal of solvent under reduced pressure (temperature <25° C.)
2. additionpentane (400 mL) and methanol (1 mL) were added
3. filtrationthe mixture filtered
4. concentrationConcentration

ORD record

ord-d0c6afc98d8743a5a17e38823fe7525c

Source dataset

uspto-grants-1998_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05854234