Preparation method of isotope 13C marked salicylic acid
A technology of isotope labeling and salicylic acid, which is applied in the direction of carboxylate preparation, organic compound preparation, isotope introduction into organic compounds, etc., can solve problems such as not involving isotope labeling, large amount of labeled carbon dioxide, and increased production costs, and achieve Fewer by-products, simple operation, and high yield
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0028] isotope 13 The preparation method of C marked salicylic acid adopts the following steps:
[0029] in N 2 Under protection, 45mmol of o-methoxybromobenzene and 0.45mmol of methyl iodide were dissolved and mixed with 200ml of anhydrous ether (dehydrated with sodium silk), and a small amount of liquid was added dropwise into a three-necked reaction flask with 1.08g of magnesium chips. via N 2 Replacement was performed 3 times, and after the reaction was initiated, the reaction solution was slowly added dropwise. The reaction temperature was maintained at 30° C., and the reaction time was 8 hours until the magnesium chips disappeared, and the reaction ended.
[0030] Use a low-temperature cooling circulation pump to reduce the reaction temperature to -30°C, and feed 13 CO 2 Gas 0.2L, the reaction liquid is milky white, absorbing 13 CO 2 Gas time 1h.
[0031] Add 10mol / L hydrochloric acid dropwise for hydrolysis, stir magnetically until the solution is transparent an...
Embodiment 2
[0034] isotope 13 The preparation method of C marked salicylic acid adopts the following steps:
[0035] in N 2 Under protection, 45mmol of o-methoxybromobenzene and 45mmol of 1,2-dibromoethane were dissolved and mixed in 200ml of tetrahydrofuran (dehydrated with sodium silk), and a small amount of liquid was added dropwise into a three-necked reaction flask with 3.24g of magnesium chips. via N 2 Replacement was performed 3 times, and after the reaction was initiated, the reaction solution was slowly added dropwise. The reaction temperature was maintained at 70° C., and the reaction time was 5 hours until the magnesium chips disappeared, and the reaction ended.
[0036] Use a low-temperature cooling circulation pump to lower the reaction temperature to -10°C, and feed 13 CO 2 Gas 1L, the reaction liquid is milky white, absorbing 13 CO 2 Gas time 6h.
[0037] Add 1mol / L sulfuric acid dropwise for hydrolysis, stir magnetically until the solution is transparent and clear,...
Embodiment 3
[0040] isotope 13 The preparation method of C marked salicylic acid adopts the following steps:
[0041] in N 2 Under protection, 45mmol of o-methoxybromobenzene and 10mmol of 1,2-dichloroethane were dissolved and mixed in 200ml of tetrahydrofuran (dehydrated with sodium wire), and a small amount of liquid was added dropwise into a three-necked reaction flask with 2.16g of magnesium chips. via N 2 Replacement was performed 3 times, and after the reaction was initiated, the reaction solution was slowly added dropwise. The reaction temperature was maintained at 50° C., and the reaction time was 2 hours until the magnesium chips disappeared, and the reaction ended.
[0042] Lower the reaction temperature to 30°C, and introduce 13 CO 2 Gas 0.5L, the reaction liquid is milky white, absorbing 13 CO 2 Gas time 3h.
[0043] Add 5mol / L acetic acid dropwise for hydrolysis, stir magnetically until the solution is transparent and clear, extract with chloroform (3×50ml), wash the o...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More