(E)-3-DIMETHYLAMINO-1-THIOPHEN-2-YL-PROPENONE synthesis
- Product Name:(E)-3-DIMETHYLAMINO-1-THIOPHEN-2-YL-PROPENONE
- CAS Number:34772-98-0
- Molecular formula:C9H11NOS
- Molecular Weight:181.25
Yield:34772-98-0 98%
Reaction Conditions:
in xylene at 130; for 48 h;Heating / reflux;
Steps:
001
2-acetylthiophene (8.20 g) and N,N-dimethylformamide diethyl acetal (13.6 mL) were heated to reflux at 130°C in xylene (13 mL) for two days. The reaction liquid was concentrated under reduced pressure, and after subjected to azeotropic distillation with toluene, crystallized with a mixed solvent of toluene-hexane and 3-dimethylamino-1-thiophen-2-ylpropenone (11.52g, yield 98%) was obtained. The obtained 3-dimethylamino-1-thiophen-2-ylpropenone (10.78 g) was dissolve in toluene (160 mL) and stirred at 100°C with 3,5-diamino-1,2,4-triazole (14.15 g) added. After 10-camphor sulfonic acid (13.82 g) was added, it was heated to reflux for 1.5 hours. After having cooled to room temperature, the supernatant was removed (decantation). The residue was suspended and washed with 5% sodium carbonate/10% ethanol aqueous solution, 10% ethanol water, absolute ethanol and methylene chloride in this order and dried under reduced pressure and the title compound was obtained (8.55 g, yield 66%).
References:
EP1674454,2006,A1 Location in patent:Page/Page column 19
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