Reacción #66366
ord-b5206da13d364368be9ce207f1374977
Ecuación de reacción
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Temperatura
60°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1ConcentraciónThe suspension was concentrated to about ¼ of the original volume
- 2workup.ADDITIONdiluted with THF (50 mL)
- 3workup.STIRRINGstirred for 5 minutes
- 4FiltraciónThe yellow solid was filtered
- 5Lavadowashed with THF
- 6Otrodried at 50° C. for 1 hours
- 7OtroThe crude product (4.59 g) was used in the following step without further purification
Procedimiento
3-(2-[1,3]Dithietan-2-ylidene-2-pyridin-4-yl-acetyl)-benzonitrile (5 g, 16.1 mmol) was suspended in absolute ethanol (50 mL) and heated to 60° C. Hydrazine monohydrate (3.13 mL, 64.4 mmol, 4 eq) was added dropwise and the mixture was stirred at 60° C. for 2 hours. The suspension was concentrated to about ¼ of the original volume, diluted with THF (50 mL) and stirred for 5 minutes. The yellow solid was filtered, washed with THF and dried at 50° C. for 1 hours. The crude product (4.59 g) was used in the following step without further purification.