Hydrazine hydrate (1:1) → 848252-38-0

Temperature

50 °C

400 mg of 2-chloro-4-methyl-3-trifluoroacetylaminothiophene were admixed with 1.5 ml of hydrazine hydrate and then stirred at 50° C. for one hour. The mixture was admixed with water, the solution was extracted using ethyl acetate and the organic phase was washed once with dilute acetic acid and once more with water. After the organic phase had been dried over sodium sulfate, it was made strongly acidic using hydrogen chloride-saturated diethyl ether, and the solvent was distilled off on a Rotavapor under reduced pressure. After distilling off to a substantial extent, the mixture was admixed again with ethyl acetate and the solvent was again distilled off, in the course of which brown-colored crystals separated out. The solid was filtered off rapidly and transferred to a desiccator for drying over diphosphorus pentoxide.

1. extractionthe solution was extracted
2. washthe organic phase was washed once with dilute acetic acid and once more with water
3. dry with materialAfter the organic phase had been dried over sodium sulfate, it
4. distillationthe solvent was distilled off on a Rotavapor under reduced pressure
5. distillationAfter distilling off to a substantial extent
6. distillationthe solvent was again distilled off, in the course of which brown-colored crystals
7. customseparated out
8. filtrationThe solid was filtered off rapidly
9. customtransferred to a desiccator
10. dry with materialfor drying over diphosphorus pentoxide

ORD record

ord-5b6d798c893d4d04aed5d0f8add2d5aa

Source dataset

uspto-grants-2007_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07179830B2