Hydrochloric Acid → 6-Fluoroisatin

温度

50 °C

9.6 g of 3-fluoroaniline were added to 590 mL of water followed by the addition of 17.2 g of trichloroacetaldehyde monohydrate, 21.9 g of hydroxyamine hydrochloride and 98.2 g of anhydrous sodium sulfate and stirring the mixture for 5 hours at 50° C. After cooling the resultant to room temperature and allowing to stand overnight, 31 mL of 2 N HCl were added thereto followed by stirring the mixture for 30 minutes and then filtering out the crystals. After drying the resulting crystals, the crystals were added to concentrated sulfuric acid heated to 70° C., followed by stirring the mixture for 1 hour at 80° C. to 90° C. The reaction mixture was poured over ice followed by extracting with ethyl acetate and washing with saturated saline. After drying the organic layer with magnesium sulfate, the solvent was distilled off under reduced pressure to obtain 7.96 g of a crude product of 6-fluoroisatin.

1. temperatureAfter cooling the resultant to room temperature
2. waitto stand overnight
3. stirringby stirring the mixture for 30 minutes
4. filtrationfiltering out the crystals
5. customAfter drying the resulting crystals
6. additionthe crystals were added to concentrated sulfuric acid
7. temperatureheated to 70° C.
8. stirringby stirring the mixture for 1 hour at 80° C. to 90° C
9. additionThe reaction mixture was poured over ice
10. extractionby extracting with ethyl acetate
11. washwashing with saturated saline
12. dry with materialAfter drying the organic layer with magnesium sulfate
13. distillationthe solvent was distilled off under reduced pressure

ORDレコード

ord-c7705bb9dc7b4dadaafb843cfd2b0be9

出典データセット

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09060517B2