反应详情

温度

20 °C

A mixture of 50.5 g (430 mmol) of 32% hydrochloric acid and 50 ml of water was added to 32.0 g (103 mmol) of (S)-4-formyl-1-(trifluoroacetyl) piperazine-2-carboxylic acid tert-butylamide in 200 ml of acetone and the resulting mixture was heated at 60° to 65° C. for 2.5 hours. After cooling to 20° C., neutralization was carried out with triethylamine in such a way that the temperature remained below 30° C. The solvent was evaporated off, and 100 ml of water and 200 ml of methyl isobutyl ketone were added. At 50° C. the phases were separated and the aqueous phase was re-extracted with twice 100 ml of methyl isobutyl ketone. The combined organic extracts were dried over magnesium sulfate and evaporated to dryness to give 23.5 g (80%) of the title compound in the form of a slightly reddish solid. Recrystallization from toluene/diisopropyl ether gave the title compound in the form of a white crystalline powder. The melting point of the title compound was: 143.5° to 144.2° C. Other data concerning the title compound was:

1. temperaturethe resulting mixture was heated at 60° to 65° C. for 2.5 hours
2. customremained below 30° C
3. customThe solvent was evaporated off
4. addition100 ml of water and 200 ml of methyl isobutyl ketone were added
5. customAt 50° C. the phases were separated
6. extractionthe aqueous phase was re-extracted with twice 100 ml of methyl isobutyl ketone
7. dry with materialThe combined organic extracts were dried over magnesium sulfate
8. customevaporated to dryness