反应详情

A mixture of 2-(tert-butyl-dimethyl-silanyloxymethyl)-4-trimethylsilanylethynyl-tetrahydro-pyran-4-ol (1.75 g, 5.1 mmol) and K2CO3 (1.4 g, 10.2 mmol) was stirred at room temperature for 30 minutes. After concentration, the residue was partitioned between EtOAc (50 mL) and water (30 mL) and the separated aqueous layer was extracted with EtOAc. The combined organic extract was dried over sodium sulfate and concentrated to give 1.33 g (96%) of light yellow oil: 1H NMR (CDCl3) δ 0.05 (s, 6H), 0.88 (s, 9H), 1.50 (m, 1H), 1.78 (m, 1H), 1.84 (d, 1H), 2.01 (m, 1H), 2.55 (s, 1H), 3.55-3.70 (m, 4H), 4.00 (m, 1H).

1. concentrationAfter concentration
2. customthe residue was partitioned between EtOAc (50 mL) and water (30 mL)
3. extractionthe separated aqueous layer was extracted with EtOAc
4. extractionThe combined organic extract
5. dry with materialwas dried over sodium sulfate
6. concentrationconcentrated
7. customto give 1.33 g (96%) of light yellow oil