反应详情

温度

5 °C

1.0 g (4.1 mmol) of (5-Hydroxyimino-5H-thiophen-2-ylidene)-(2-methylphenyl)-acetonitrile, prepared as described in example 7.1, are dissolved in 11 ml of THF and cooled in an ice bath. After adding 0.83 g (4.5 mmol) of trichloroacetyl chloride to the solution, 0.63 g (6.2 mmol) of triethylamine are added dropwise, keeping the temperature below 5° C. While the reaction mixture is stirred at 5° C. for 20 min, a precipitate is formed. The precipitate is filtered off and washed with THF. The filtrate is concentrated by a rotary evaporator. The residue is diluted with 2-PrOH and stirred at room temperature for 15 min. After cooling the mixture in an ice bath, the solid is isolated by filtration and washed with 2-PrOH. The product is obtained in the form of a yellow solid, 165° C.(Dec). The structure is confirmed by the 1H-NMR spectrum (CDCl3). δ [ppm]: 2.39 (s, 3H), 6.23 (d, 1H), 6.86 (d, 1H), 7.19-7.4 (m, 4H).

1. temperaturecooled in an ice bath
2. additionare added dropwise
3. customthe temperature below 5° C
4. customa precipitate is formed
5. filtrationThe precipitate is filtered off
6. washwashed with THF
7. concentrationThe filtrate is concentrated by a rotary evaporator
8. additionThe residue is diluted with 2-PrOH
9. stirringstirred at room temperature for 15 min
10. temperatureAfter cooling the mixture in an ice bath
11. customthe solid is isolated by filtration
12. washwashed with 2-PrOH
13. customThe product is obtained in the form of a yellow solid, 165° C.(Dec)