Ammonium Hydroxide → 5-Bromo-1,3,4-thiadiazole-2-carboxamide

To a solution of ethyl 5-bromo-1,3,4-thiadiazole-2-carboxylate (13.5 g, 56.9 mmol) in THF (50 mL) at room temperature was added NH4OH (28 wt. %, 39.6 mL, 164 mmol). The mixture was stirred at room temperature overnight and a precipitate appeared in the aqueous layer. Volatile materials were removed in vacuo. The mixture was diluted with water and the precipitate was collected, washed with water and dried under vacuum to give the title compound. 1H NMR (400 MHz, acetone-d6): δ7.99 (s, 1H), 7.55 (s, 1H).

1. customVolatile materials were removed in vacuo
2. additionThe mixture was diluted with water
3. customthe precipitate was collected
4. washwashed with water
5. customdried under vacuum

ORD record

ord-3f6697c223e34916bedf03631935459f

Source dataset

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08063224B2