反应详情

温度

120 °C

2-Amino-5-bromo-terephthalic acid dimethyl ester (15.0 g, 52.1 mmol), zinc (II) cyanide (6.11 g, 52.1 mmol) and tetrakis(triphenylphosphine)palladium (0) (3.0 g, 2.6 mmol) were suspended in DMF (50 ml) and the resultant reaction mixture degassed was purged with argon. The reaction mixture was heated at 120° C. for 30 minutes then concentrated in vacuo. The resultant residue was triturated with hot water (100 ml) and the product collected by filtration to yield the title compound as a dark grey solid (12.0 g, 98%). 1H NMR (d6-DMSO, 400 MHz) 8.11 (1H, s), 7.62 (2H, br s), 7.52 (1H, s), 3.89 (3H, s), 3.85 (3H, s).

1. customthe resultant reaction mixture
2. customdegassed
3. customwas purged with argon
4. concentrationthen concentrated in vacuo
5. customThe resultant residue was triturated with hot water (100 ml)
6. filtrationthe product collected by filtration