A kind of deacetyllanatoside crystal form and preparation method thereof
A technology of acetyl lanatoside crystals and deacetyl lanatoside, which is applied in the field of deacetyl lanatoside crystal form II and its preparation, and can solve the problem of less deacetyl lanatoside crystal forms and no deacetyl lanatoside crystal forms etc. to achieve the effects of high product purity, simple preparation method and high yield
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0033] Example 1: Preparation of deacetyl lanolin II crystal form
[0034] Add 5.0g of deacetyl lanolin to the reaction flask, then add 30mL of isopropanol, stir well, heat up to 65℃, then add 1mL of deionized water dropwise, keep the temperature and stir for 3h, then cool to 30℃ naturally, filter by suction, filter After the cake was rinsed and drained with a small amount of isopropanol, it was transferred to a drying oven at 60-65°C and vacuum dried for 6 hours to obtain 4.7 g of white solid. The yield of deacetyl lanolin was 94.0%, the moisture content was 0.27%, and the related substances: the largest single impurities were 0.22%, and the total impurities were 0.65%. Use Cu-Ka radiation to obtain the X-ray powder diffraction spectrum expressed in 2θ angles. figure 1 , At 8.25±0.2°, 10.44±0.2°, 11.63±0.2°, 12.74±0.2°, 13.12±0.2°, 14.59±0.2°, 15.46±0.2°, 16.73±0.2°, 18.78±0.2°, 19.55±0.2 °、20.44±0.2°、21.07±0.2°、21.63±0.2°、22.03±0.2°、22.53±0.2°、23.38±0.2°、24.67±0.2°、25.15±0.2°、...
Embodiment 2
[0035] Example 2: Preparation of crystalline form of deacetyl lanolin II
[0036] Add 5.0g of deacetyl lanolin to the reaction flask, then add 30mL of isobutanol, stir well, heat up to 65℃, then add 1mL of deionized water dropwise, keep warm and stir for 3h, then cool to 30℃ naturally, filter with suction, filter After the cake was rinsed and drained with a small amount of isobutanol, it was transferred to a drying oven at 60-65°C and vacuum dried for 6 hours to obtain 4.8 g of white solid. The yield of deacetyl lanolin was 96.0%, the moisture was 0.29%, and the related substances: the largest single impurities were 0.21%, and the total impurities were 0.67%.
Embodiment 3
[0037] Example 3: Comparative example. The preparation method of the prior art product refers to Chinese patent CN 104447933 A to obtain desacetyl lanolin crystal form I. Using Cu-Ka radiation, the X-ray powder diffraction spectrum expressed in 2θ angles is obtained, see Attached image 3 .
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More