2,2,2-Trifluoroethanol → 2,2,2-Trifluoroethyl trifluoroacetate

After five cycles similar to the one described above, the gas chromatographic analysis showed only 80% conversion to trifluoroethanol and the catalyst was then regenerated in the following manner. The pressure tube containing the catalyst residue (originally 0.03 mmol) was charged with 20 mg (0.25 mmol) of NaBH(OCH3)3, in a dry box. Tetrahydrofuran (3 ml) was distilled into the tube under vacuum and the solution stirred at room temperature for one hour. The solvent and other volatiles were removed in vacuo and the residue evacuated to dryness. The pressure tube was then charged with toluene (3 ml) and 1.1 gram (5.7 mmols) of ester and the hydrogenation was conducted as described in part (a).

1. additionThe pressure tube containing the catalyst residue (originally 0.03 mmol)
2. distillationTetrahydrofuran (3 ml) was distilled into the tube under vacuum
3. customThe solvent and other volatiles were removed in vacuo
4. customthe residue evacuated to dryness

ORD record

ord-a7736cb0dcc34e01b6534daadc1fc7f4

Source dataset

uspto-grants-1980_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04232170