sensor
A sensor and container technology, applied in the field of stent sensors, can solve the problems of bacteria affecting normal tissues and drug waste.
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Embodiment 1
[0164] Example 1: Synthesis of all cis-5-((tert-butyldimethylsilyl)oxy)cyclohexane-1,3-diol (1):
[0165] Add all-cis-cyclohexane-1,3,5-triol (100 mg, 0.757 mmol) (dried at 110 °C for 3 h under high vacuum to remove crystallization water) in 2 ml of dry THF (tetrahydrofuran) at room temperature TBS-Cl (tert-butyldimethylsilyl chloride) (125mg, 0.832mmol) and triethylamine (0.086ml, 0.616mmol) were added successively to the suspension. Then a portion of NaH (36.3 mg, 0.832 mmol) was added. The mixture was heated to 40 °C over 30 min and stirred at 40 °C for 2 h. The suspension was cooled to 8°C and filtered. The filtrate was evaporated. The residue was triturated in 1 ml of hexane at room temperature and filtered. The filtrate was dried under high vacuum overnight to afford (1) (111 mg, 0.450 mmol, 59% yield) as a white solid.
Embodiment 2
[0166] Example 2: Synthesis of (1R,3S,5S)-3-((tert-butyldimethylsilyl)oxy)-5-hydroxycyclohexyl acetate (2):
[0167] 1 (3.660g, 14.85mmol) was dissolved in vinyl acetate (37.0ml, 401mmol) and 350ml of ethyl acetate. Amano lipase SP (1 g, 0.00 μmol) from Burkholderia cepacia was added, and the mixture was stirred at room temperature for 10 days. The enzyme was filtered off, the filtrate was concentrated and the residue was dried under high vacuum overnight to afford 2 (2.356 g, 8.17 mmol, 55% yield) as a yellowish oil.
Embodiment 3
[0168] Example 3: Synthesis of (4-((trimethylsilyl)ethynyl)phenyl)methanol (3):
[0169] 4-Bromobenzyl alcohol (1.276g, 6.82mmol), trimethylsilylacetylene (1.061ml, 7.51mmol), PdCl 2 (PPh 3 ) 2 (24mg, 0.034mmol), copper iodide (52mg, 0.273mmol), triphenylphosphine (358mg, 1.365mmol), diethylamine (10.70ml, 102mmol) in 2ml dry DMF (dimethylformamide) solution Heat at 150 °C for 30 min in a microwave oven under argon. Filter the mixture. The filtrate was acidified with 1M HCl and extracted 3 times with ether. The combined organic layers were washed with bicarbonate and water, washed with MgSO 4 Drying and concentration afforded 3 (1.274 g, 6.23 mmol, 91% yield) as a tan solid.
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