二叔丁亚甲硅基是有机合成中非常有用的双官能团硅醚。常用的制备试剂有(t-Bu)₂SiCl₂,(t-Bu)₂Si(OTf)₂。脱保护试剂有48% aq HF；TBAF；HF-pyridine；TASF等，这和普通硅醚的脱保护类似。

制备示例 (Org. Lett. 2011, 13, 3446)

To a cloudy solution of 1 (690 mg, 1.95 mmol) in DMF (15 mL) at 0°C was added di-tert-butylsilyl-bis(trifluoromethanesulfonate) (0.81 mL, 1.1equiv). After stirring at 0 °C for 10 min, ice-water bath was removed to allow the temperature going back tort. Imidazole (332 mg, 2.5 equiv) was then added and the mixture was stirred atrt for 0.5 h. After removal of DMF under high vacuum, the residue was dissolved in ethyl acetate, washed with water, 5% NaHCO₃ solution and brine, and dried over Na₂SO₄. After evaporation of the solvent under reduced pressure, the residue was purified by silica gel chromatography, eluting with 3-6% MeOH in CH₂Cl₂, to give 2 (913mg, 95%) as a white foam.

脱保护示例 (Synthesis, 2010, 2708)

HF·pyridine(0.300 mL, 2.07 mmol) was carefully diluted with pyridine (0.50 mL) and then added dropwise to a solution of 1 (229 mg, 0.41 mmol) in THF (6 mL) at 0 °C. The mixture was warmed to r.t. and stirred for 10 min. TLC showed that the reaction was complete. The mixture was diluted with pyridine (2 mL). This mixture was partitioned between CH₂Cl₂ and H₂O, and the organic layer was washed with 5% NaHCO₃ solution and brine, then dried (anhydrous Na₂SO₄). The solvent was removed, and the residue was purified by silica gel chromatography(MeOH:CH₂Cl₂, 4:96), affording 2 (156 mg, 91%) as a white foam.

此类硅醚衍生物通常由1,3-dichloro-1,1,3,3-tetraisopropyldisiloxane(TIPDS-Cl₂)制备得到。脱保护常用的试剂有TBAF，HF-TEA，NH₄F等。

制备示例 (Chem. Eur. J. 2008, 14,11194)

Diol 1 (515mg, 1.56 mmol) was subjected to coevaporation of the volatiles with anhydrous pyridine three times, and then suspended in anhydrous pyridine (10 mL) under anitrogen atmosphere. 1,3-Dichloro-1,1,3,3-tetraisopropyldisiloxane (TIPDS-Cl₂)(530 mL, 526 mg, 1.67 mmol) was then added and the reaction mixture was stirred for 16 h at room temperature. The reaction was stopped by the addition of methanol (1 mL). The mixture was diluted with dichloromethane and washed once with water and once with brine. The solvent was removed in vacuo, and the residue was purified by flash chromatography on silica gel (5% MeOH in CH₂Cl₂) and recrystallized from hexane to give 2 as a colorless solid (880 mg, 1.54 mmol, 98%).

脱保护示例 (Helv. Chim. Acta, 2011, 94, 362)

To a solution of 1(8.0 g, 10.5mmol) in THF (70 ml) was added Bu₄NF·3H₂O (8.0 g, 25.4 mmol) in THF (80 ml) with stirring. After 10 min, the mixture was neutralized by AcOH (9.2 ml, 154.4mmol) in THF (30 ml) and concentrated. The residue was dissolved in CHCl₃(500 ml), the solution washed with NaHCO₃ solution (200 ml) and H₂O(100 ml), dried (Na₂SO₄), and concentrated, and the residue crystallized from EtOH to give 2 (6.2 g, 88%).