Stannous Chloride → 5-Bromo-2,3-diaminobenzotrifluoride

Temperatur

90 °C

To a stirred mixture of 2-amino-5-bromo-3-nitrobenzotrifluoride (261 mg, 0.949 mmol) in ethanol (4 mL) was added SnCl2 ·2H2O (1.076 g, 4.745 mmol) in one portion. The mixture was refluxed at 80° C. (oil bath 90° C.) for 1 h. The solution was cooled to room temperature and ice water (20 g) was added. It was adjusted to pH=7 with NaHCO3 and extracted by ethyl acetate (2×4 mL). The extract was dried over Mg2SO4 and evaporated to give 150 mg (64.6%) of 2,3-diamino-5-bromobenzotrifluoride as a brown solid. 1H NMR (CDCl3): δ3.503 (s, 2H); 3.898 (s, 2H); 6.987 (d, 1H, J=1.8 Hz); 7.123 (d, 1H, J=1.8 Hz).

1. temperatureThe solution was cooled to room temperature
2. extractionextracted by ethyl acetate (2×4 mL)
3. dry with materialThe extract was dried over Mg2SO4
4. customevaporated

ORD-Eintrag

ord-6a5028df2d894647a22b7afa91595ab5

Quelldatensatz

uspto-grants-1996_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05514680