4-(CHLOROMETHYL)-2-(4-METHOXYPHENYL)-1,3-THIAZOLE HYDROCHLORIDE synthesis
- Product Name:4-(CHLOROMETHYL)-2-(4-METHOXYPHENYL)-1,3-THIAZOLE HYDROCHLORIDE
- CAS Number:23421-57-0
- Molecular formula:C11H10ClNOS
- Molecular Weight:239.72
Yield:23421-57-0 82%
Reaction Conditions:
Stage #1: p-methoxythiobenzamide;1,3-Dichloroacetone in chlorobenzene at 20; for 6 h;
Stage #2: in methanol; for 5 h;
Steps:
3
Then, the solution of the monochlorobenzene 92.7g in which 78.5 g (0.62 mol) of 1,3-dichloroacetone was dissolved for the monochlorobenzene 160g after addition was dropped over 2 hours at 20 degrees C, and was agitated for 4 hours. Then, the methanol 61.8g was dropped over 1 hour. It agitated for further 4 hours, cooled to the room temperature after checking ending reaction using HPLC, and carried out decompression distilling off of the monochlorobenzene after washing with a 15 mass % potassium carbonate aqueous solution and water. It is the 4-chloromethyl 2 by filtering and drying in vacuum the crystal obtained by adding and recrystallizing 556.1 g of heptane. -(4-methoxy-phenyl)- 121.5 g (0.51 mol) of thiazoles were acquired in the HPLC purity 99.8 area %. Obtained 4-chloromethyl 2 -(4-methoxy-phenyl)- The yield of the thiazole was 82% to 4-methoxybenzo nitrile.
References:
JP2015/107948,2015,A Location in patent:Paragraph 0081
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