反应详情

温度

120 °C

The reaction was carried out in 4 batches using ACE pressure tubes. The 4-amino-3-(tetrahydrofuran-3-yloxy)-benzamide (0.52 g, 1.0 eq, 2.34 mmol) was added to a solution of 4-chlorothieno[3,2-d]pyrimidine (0.40 g, 1.0 eq, 2.34 mmol) in IPA (4 ml). The reaction mixtures were then stirred at 120° C. for 18 hours before being allowed to cool. 28% w/w Ammonium hydroxide solution (4 ml) followed by water (8 ml) were added and the reactions combined. The precipitate was isolated by filtration, washed with water (4×50 ml), dried on the sinter, washed with cyclohexane (8×50 ml), and then dried in vacuo to give the title compound as an off-white solid (2.71 g, 7.6 mmol, 81%). LCMS: [M+H]+=357; Rt=1.27 min, 100% purity.

1. customThe reaction mixtures
2. temperatureto cool
3. additionwere added
4. customThe precipitate was isolated by filtration
5. washwashed with water (4×50 ml)
6. customdried on the sinter
7. washwashed with cyclohexane (8×50 ml)
8. customdried in vacuo