Acetic Acid → 6-(4-Bromo-phenyl)-4,7-dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalene

5-(4-Bromo-benzoyl)-5,6-dihydro-cyclopenta[b]thiophen-4-one (8.0 g, 25 mmol), hydrazine monohydrate (4.8 mL, 150 mmol), glacial acetic acid (1.8 mL) and ethanol (45 mL) was heated at 100° C. under nitrogen for 4 hr. The mixture was cooled to 25° C. and concentrated under reduced pressure to give a solid which was recrystallized from ethanol to provide the corresponding 6-(4-Bromo-phenyl)-4,7-dihydro-1-thia-4,5-diaza-cyclopenta[a]pentalene (7.6 g, 24.2 mmol) as white solid in 97% yield.

1. concentrationconcentrated under reduced pressure
2. customto give a solid which
3. customwas recrystallized from ethanol

ORD-Eintrag

ord-1fb2ec85110040048c3eadc934c8c69d

Quelldatensatz

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08853207B2