Compound manufacturing method, compound, and mixture
A manufacturing method and compound technology, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc.
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0206] The mixture 1 containing the intermediate compound (1) and the compound (2) was produced according to the following scheme. In addition, in the following scheme, "NMP" means N-methyl-2-pyrrolidone, and "AcOH / AcONa Buffer" means an acetic acid-sodium acetate buffer solution.
[0207]
[0208]
[0209] In a 3-port reactor with a thermometer, 41.2 g (239 mmol) of trans-1,4-cyclohexanedicarboxylic acid, 100 g of N-methyl-2- Pyrrolidone (NMP) to give a solution. To the obtained solution, 12.64 g (47.83 mmol) of the hydroxy compound represented by the formula (A), 4-(6-acryloyloxy-hex-1-yloxy)phenol (manufactured by DKSH), 643 mg (5.26 mmol) were added. mmol) of 4-(dimethylamino)pyridine as base. To this solution, 11.0 g (57.4 mmol) of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride as a condensing agent was slowly added dropwise over 1 hour. Then, the whole content was stirred for 15 hours, and the esterification reaction was performed at room temperature...
Embodiment 2
[0217] A reaction solution was obtained by changing to a synthesis method using trans-1,4-cyclohexanedicarboxylic acid dichloride instead of trans-1,4-cyclohexanedicarboxylic acid as a raw material, and an intermediate compound containing ( 1) and a mixture 2 of compound (2). The reaction scheme is as follows. In addition, in the following scheme, "THF" means tetrahydrofuran.
[0218]
[0219]
[0220] First, in a 3-port reactor equipped with a thermometer, 10.0 g (47.83 mmol) of trans-1,4-cyclohexanedicarbonyl dichloride and 100 ml of tetrahydrofuran as a hydrophilic organic solvent were added in a nitrogen stream. (THF). To this, 12.04 g (45.55 mmol) of 4-(6-acryloyloxy-hex-1-yloxy)phenol (manufactured by DKSH) was added as a hydroxy compound, the reactor was immersed in a water bath, and the reaction solution was immersed. The temperature was set to 0°C. Next, 4.83 g (47.83 mmol) of triethylamine as a base was slowly added dropwise over 5 minutes while keeping the in...
Embodiment 3
[0228] The mixture 3 containing the intermediate compound (1) and the compound (2) was produced according to the following scheme. In this example, a mixture 3 was produced through the same process (B1) as the process (A1) in Example 1, the processes (B2) and (B3) described in detail below, and the first and second filtration and washing processes. . In addition, in the following scheme, "NaOHaq." means sodium hydroxide aqueous solution, and "HClaq." means hydrochloric acid aqueous solution.
[0229]
[0230]
[0231] In a 3-port reactor with a thermometer, 41.2 g (239 mmol) of trans-1,4-cyclohexanedicarboxylic acid, 100 g of N-methyl-2- Pyrrolidone (NMP) to give a solution. To the obtained solution, 12.64 g (47.83 mmol) of 4-(6-acryloyloxy-hex-1-yloxy)phenol (manufactured by DKSH), a hydroxy compound represented by the formula (A), and 643 mg (5.26 mmol) were added. mmol) of 4-(dimethylamino)pyridine as base. To this solution, 11.0 g (57.4 mmol) of 1-(3-dimethylamino...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More