In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 4584-46-7 as follows. HPLC of Formula: C4H11Cl2N
Provided in is step-by-step synthesis of PCA 1 and PCA 2. To make intermediate 3a 4-(2-(dimethylamino)ethoxy)-3-methoxybenzaldehyde, vanillin (1.52 g, 10 mmol), 2-chloro-dimethylethylamine HCI (2.16 g, 15 mmol), potassium iodide (332 mg, 2 mmol) and potassium carbonate (4.14 g, 30 mmol) were suspended in acetone and heated at reflux for 16 h. Next, volatiles were removed in vacuo and the resulting residue is redissolved in water and ethyl acetate. The organic layer was separated and washed with brine and dried with magnesium sulfate. Concentrating in vacuo resulted in 1.75 g (78%) of a yellow oil. NMR and mass spectrometry analysis of intermediate 3a 4-(2-(dimethylamino)ethoxy)-3-methoxybenzaldehyde is provided in to 4C: 1H NMR (400 MHz, Chloroform-d) delta9.82 (s, 1H), 7.41 (dd, J=8.2, 1.9 Hz, 1H), 7.37 (d, J=1.9 Hz, 1H), 6.96 (d, J=8.2 Hz, 1H), 4.17 (t, J=6.1 Hz, 2H), 3.89 (s, 3H), 2.79 (t, J=6.1 Hz, 2H), 2.32 (s, 6H). () 13C NMR (101 MHz, CDCl3) delta191.2, 154.0, 150.0, 130.3, 127.0, 111.7, 109.3, 67.4, 58.0, 56.2, 46.3. () ESI-MS [M+H]: Calculated: 224.1; Observed: 224.1 ()
According to the analysis of related databases, 4584-46-7, the application of this compound in the production field has become more and more popular.
Reference:
Patent; The Board of Trustees of the Leland Stanford Junior University; Velema, Willem Arend; Kool, Eric T.; (79 pag.)US2019/264205; (2019); A1;,
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