Aluminium lithium hydride → HCID 57025985, compound

Participants

Reaction Conditions

Reaction Steps

To a suspension of lithium aluminium hydride (63 mg, 1.65 mmol) in ether (10 ml) the difluoroester (6) (1.40 g, 2.76 mmol) in ether (10 ml) was added and the mixture was stirred at 0° C. for 10 min and then stirred at room temperature for 10 min. The usual work-up (ether for extraction) gave a crude product, which was applied to a column of silica gel (100 g). Elution with n-hexane-ether (5:1) gave the alcohol (7) (1.13 g, 86%), viscous oil. 1H-NMR δ: 0.73 (3H, s, 18-H3), 1.03 (3H, s, 19-H3), 1.13 (3H, d, J=6 Hz, 21-H3), 3.33-4.10 (5H, m, 24-H2, 3-H, and THP), 4.76 (1H, m, THP), 5.38 (1H, m, 6-H). 19F-NMR δ: +43.3. MS m/z: 396 (M+ -DHP), 378.

Provenance & Evidence