Method for producing diarylpyridine derivatives
A manufacturing method, dimethylformamide technology, applied in the manufacturing field, can solve problems such as difficult operation
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment
[0075] Hereinafter, the present invention will be further described in detail by way of examples, but the scope of the present invention is not limited thereto.
[0076] The symbols used in the examples have the following meanings.
[0077] mg: milligram; g: gram; kg: kilogram; mL: milliliter; L: liter;
[0078] mol: mole; MHz: megahertz.
[0079] In the following examples, the nuclear magnetic resonance (hereinafter referred to as 1H NMR: 500 MHz) spectrum uses tetramethylsilane as a standard substance, and the chemical shift values are expressed in δ values (ppm). The singlet of the splitting pattern is represented by s, the doublet is represented by d, the triplet is represented by t, the quartet is represented by q, the multiplet is represented by m, and the broad peak is represented by br.
[0080] The detection conditions of the X-ray powder diffractometer used in the examples are as follows.
[0081] Detection range: 3-40deg
[0082] Step size: 0.020deg
[0083...
reference example 1
[0089] Preparation of (5-methylpyridin-2-yl)potassium acetate (2)
[0090]
[0091] Under a nitrogen atmosphere, ordinary water (25.7 L) and (5-methylpyridin-2-yl)acetic acid hydrochloride (1) (19.0 kg, 101 mol) were added to the reaction vessel, and stirred at 0°C. After adding 48% aqueous potassium hydroxide solution (23.24 kg) while keeping the temperature at -5°C or higher and 10°C or lower, the pH was adjusted to 12.6 with concentrated hydrochloric acid (0.15 kg). After confirming the precipitation of potassium chloride, the mixture was stirred at 0° C. for 20 minutes, and 1-propanol (143 L) was added dropwise. After the dropwise addition, the temperature was raised to 25° C. and stirred for 15 minutes, and concentrated under reduced pressure to a liquid volume of 66.5 L. 1-Propanol (143L) was added dropwise at 20°C, and concentrated under reduced pressure again to a liquid volume of 66.5L. Then, 1-propanol (143 L) was added dropwise at 25° C., and after hot filtrati...
reference example 2
[0094] Preparation of (5-methylpyridin-2-yl)potassium acetate (2)
[0095]
[0096] Under a nitrogen atmosphere, toluene (315 mL), 2-fluoro-4-picoline (3) (45 g, 405 mmol), and acetonitrile (20.0 g, 487 mmol) were added to a reaction vessel, followed by stirring at 0°C. A toluene solution of potassium hexamethyldisilazide (0.5 mol / L, 1.78 L, 890 mmol) was slowly added dropwise while keeping the temperature above 0°C and below 10°C. After stirring at 25°C for 1 hour, it was stirred at 50°C for 6 hours. After cooling to 5°C, ordinary water (450 mL) was added, followed by stirring for 30 minutes. Liquid separation was carried out at 5°C, and the aqueous layer was discarded. 2N Aqueous hydrochloric acid (522 mL) was added to the organic layer to adjust the pH to 2.4. After raising the temperature to 25°C and stirring for 15 minutes, the pH was adjusted to 8.7 with 4N aqueous sodium hydroxide solution. After stirring at 25°C for 15 minutes, the aqueous layer was discarded, a...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More