反应详情

To a solution of N-[2-(3-acetyl-5-chloro-2-methoxy-6-methylphenyl)-2-hydroxyethyl]-2-chloroacetamide (170 mg, 0.50 mmol) (single enantiomer from step 3) in tetrahydrofuran (4 mL) cooled at 0° C., a mixture of sodium hydride (60% dispersion in mineral oil; 39 mg, 1.0 mmol) was added and stirred for 1 hour. The reaction was quenched with water and extracted with ethyl acetate. The combined extracts were washed with brine, dried over sodium sulfate, and concentrated to give the crude residue as a single enantiomer, 61 mg, 41%. LCMS calculated for C14H17ClNO4 (M+H)+: m/z=298.1; found: 298.1.

1. additionwas added
2. customThe reaction was quenched with water
3. extractionextracted with ethyl acetate
4. washThe combined extracts were washed with brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated