Method for preparing high-purity borneol from camphor, camphor reduction product and borneol
A high-purity, camphor-based technology, used in the fields of chemistry and medicine, can solve problems such as difficult industrialization, pollution, and low yield
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Embodiment 1
[0067] Example 1 Isopropanol is an example,
[0068] Take 4g aluminum powder (AR) and add 4g anhydrous AlCl 3 (AR), mix quickly, add 200ml of isopropanol (AR), under airtight, reflux in a water bath for 12h, add 100g of borneol, in a water bath until the borneol is dissolved, shake well to form a homogeneous solution. Distill about 170 ml -180 ml of isopropanol in a gas bath at 120°C. Under airtight, react at 150°C for 15h in a gas bath, add water, and after heating for 2h, pass into steam distillation, condense, and the distillate first comes out of a liquid containing camphene and a small amount of camphene. The latter mainly contains borneol crystalline solid and a small amount of camphene. A small amount of camphene was heated to dissolve borneol, and then sublimated at 170°C-180°C to obtain 40.2g. The purity of borneol was determined by GC to be 96.8%. Based on borneol, the yield of borneol was 40.2%.
Embodiment 2
[0070] Take 4g aluminum powder (AR) and add 4g anhydrous AlCl 3 (AR), mix quickly, add 200ml of isopropanol (AR), under airtight, reflux in a water bath for 12h, add 100g of borneol, in a water bath until the borneol is dissolved, shake well to form a homogeneous solution. Distill about 170 ml -180 ml of isopropanol in a gas bath at 120°C. Under airtight, react at 150°C for 15h in a gas bath, add water, and after heating for 2h, pass into steam distillation, condense, and the distillate first comes out of a liquid containing camphene and a small amount of camphene. The latter mainly contains borneol crystalline solid and a small amount of camphene. Add a small amount of camphene and 4 times the amount of borneol to dissolve in cyclohexane, divide the upper layer solution, dry with anhydrous sodium sulfate, add 200ml DMSO (AR), evenly, place it at 10℃ for 3-4h, divide the lower layer solution Or siphon the lower layer solution, dilute with water, filter, and crystallize it once...
Embodiment 3
[0072] Take 4g aluminum powder (AR) and add 4g anhydrous AlCl 3 (AR), mix quickly, add 200ml of isopropanol (AR), under airtight, reflux in a water bath for 12h, add 100g of borneol, in a water bath until the borneol is dissolved, shake well to form a homogeneous solution. Distill about 170ml -180ml of isopropanol in a gas bath at 120°C. Under airtight, react at 150℃ for 15h in a gas bath, add water, heat for 2h, pass into steam distillation, condense, the distillate first comes out of the liquid containing camphene and a small amount of camphene, using 4 times the amount of cyclohexane The alkane is dissolved and dried with anhydrous sodium sulfate to obtain sample solution (I). The latter mainly contains borneol crystalline solid and a small amount of camphene. Add a small amount of camphene and 4 times the amount of borneol to dissolve in cyclohexane, divide the upper solution, and dry with anhydrous sodium sulfate to obtain sample solution (II). Take 350g of column chroma...
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