4-(chloromethyl)-2-[(dimethylamino)methyl]-4,5-dihydro-4-Thiazolol synthesis
- Product Name:4-(chloromethyl)-2-[(dimethylamino)methyl]-4,5-dihydro-4-Thiazolol
- CAS Number:92759-37-0
- Molecular formula:C7H13ClN2OS
- Molecular Weight:208.71
![Acetamide, 2-[(dimethylamino)thio]-](/CAS/20210305/GIF/785024-70-6.gif)
Yield: 83%
Reaction Conditions:
Stage #1:dimethylaminothioacetamide with sodium hydrogencarbonate;sodium sulfate in di-isopropyl ether at 55 - 60; for 1 h;
Stage #2:1,3-Dichloroacetone in di-isopropyl ether at 50 - 55; for 2 h;
Steps:
2 Example No: 2 Preparation of 4-CHLOROMETHYL-4-HYDROXY-2-DIMETHYLAMINOMETHYL-2- thiazoline
DIMETHYLAMINOTHIOACETAMIDE hydrochloride (1000 G, 6.472 mol) is suspended in diisopropylether (4000 RNL). Added into this suspension is sodium bicarbonate (1200 G, 14.28 mol) and sodium sulphate (1000 G). THE slurry is heated to 55-60 C and stirred for 1 hr. Into this suspension is added 1,3 dichloroacetone (1000 G, 7.87 mol) dissolved in diisopropylether (1000 ml). The reaction is continued at 50-55o C for 2 h. The progress of the reaction is monitored by a qualitative HPLC analysis. Upon completion of the reaction, the reaction mixture ISOFILTERED hot at 50-55 C to remove insoluble inorganic salts. The mother liquor is cooled slowly to 0-5 C to crystallize out the product. The product is then filtered and washed with precooled diisopropylether (250 ml). The product is dried at 50 C under reduced pressure to obtain 1120 g. Yield = 83% ; HPLC purity = 98.2%.
References:
KUMAR, Dinesh, R. WO2004/69817, 2004, A1 Location in patent:Page 7
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