Preparing method for 3-e Menthyloxy -1,2-propanediol
A technology of propylene glycol and oxypropane, which is used in the preparation of ether from alkylene oxide, the preparation of organic compounds, the preparation of ether by dehydration of hydroxyl-containing compounds, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0130] Synthesis of 1-Chloro-3-l-oxy-2-propanol
[0131] (1) In a nitrogen atmosphere, 136.7 g (0.8763 mol) of l-menth alcohol (Takasago International Corporation) and 295 ml of n-heptane were charged into a reaction flask (500 ml capacity) and dissolved at room temperature. Then, 3.5 grams (26.88 milliliters) of anhydrous aluminum chloride were added therein, stirred to dissolve it, and the solution was heated to 70° C., and 61 grams (0.6572 moles) of epichlorohydrin was added dropwise to the solution at the same temperature, and the solution was added dropwise. Add time is 2 hours. After completion of the dropwise addition, the reaction was carried out at the same temperature for 2 hours. After this time, the reaction mixture was cooled to room temperature.
[0132] (2) The reaction mixture obtained in (1) was washed with water and then with 10% aqueous sodium carbonate solution, and an oil was obtained by evaporating n-heptane. By distilling the oil under reduced pressu...
Embodiment 2
[0139] Synthesis of 1-Acetoxy-3-l-oxy-2-propanol
[0140] (1) In a nitrogen atmosphere, 20 grams of 1-chloro-3-l-menthoxyl-2-propanol (chemical purity 97.86%, 78.78 mmoles), 7.13 grams (86.92 mg mol) of anhydrous sodium acetate and 0.51 g (1.582 mmol) of tetrabutylammonium bromide were added to a reaction flask (100 ml capacity), and then reacted at 150-160° C. for 4 hours. Thereafter, the reaction mixture was cooled to 50°C or lower.
[0141] (2) The reaction mixture prepared in (1) was mixed with 30 ml of water and 50 ml of heptane for separation, the organic layer was washed with saturated brine and dried over anhydrous sodium sulfate, and then the solvent was recovered to obtain an oily substance. Partially purified 1-acetoxy-3-l-menthoxy-2-propanol obtained by distillation of this oil under reduced pressure at a boiling point of 111-120°C / 25 Pa (0.19 mmHg) . When analyzed by gas chromatography, the product composition consisted of 5.53% by mass of 3-l-menthoxyl-1,2-pr...
Embodiment 3
[0149] Synthesis of 1-formyloxy-3-l-oxy-2-propanol
[0150] The reaction was carried out under the same conditions as in Example 2, except that anhydrous sodium formate was used instead of anhydrous sodium acetate to obtain 1-formyloxy-3-l-menthoxyl-2-propane with a yield of 60.9% alcohol.
PUM
| Property | Measurement | Unit |
|---|---|---|
| optical purity | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More