Welcome to chemicalbook!
Chinese English Japanese Germany Korea
400-158-6606
Try our best to find the right business for you.
Do not miss inquiry messages Please log in to view all inquiry messages.

Welcome back!

ChemicalBook CAS DataBase List Antioxidant 1520

Antioxidant 1520 synthesis

3synthesis methods
-

Yield:110553-27-0 99.1%

Reaction Conditions:

Stage #1: formaldehyd;Octanethiol;ortho-cresolwith hydrogenchloride;2,2'-iminobis[ethanol] in water; pH=Ca. 3 - 4; for 8 h;Reflux;
Stage #2: methyl iodidewith copper(l) iodide at 95; for 4 h;Temperature;

Steps:

1-3; 1-4 Example 2

Add 216.3g (2.0mol) of o-cresol, 599.8g (4.1mol) of n-octyl mercaptan, 126.1g (4.2mol) of paraformaldehyde, 21.0g (0.2mol) of diethanolamine, and 120ml of water into the reaction kettle,Then add concentrated hydrochloric acid to adjust the pH to about 3-4, and react for about 8 hours under reflux conditions.Then the temperature was lowered to 60-70°C and left to stand for stratification, and the lower water phase was discharged from the lower outlet of the reactor.Then, 14.2 g (about 0.1 mol) of methyl iodide and 2.1 g of CuI were added, and then reheated to 95° C., and the reaction was continued for 4 hours.After the reaction, it was naturally cooled to room temperature, the insoluble matter was removed by filtration, 6 ml of formic acid was added, and the mixture was heated to 45° C. and stirred for 0.5 hour, and then washed twice with water.The washed liquid was vacuum distilled to remove residual small molecules and volatile substances under the conditions of 20mmHg vacuum/120°C, and then dried with anhydrous sodium sulfate to obtain 842.5g of a colorless, odorless and transparent solution with a yield of 99.1%.The content of 2,4-bis(n-octylthiomethylene)-6-methylphenol in the product was 99.2%, and n-octyl mercaptan was not detected.

References:

CN113045462,2021,A Location in patent:Paragraph 0004; 0037-0038; 0039-0040; 0041-0042; 0043-0044

Antioxidant 1520 Related Search: