反应详情

温度

40 °C

To (S)-tert-butyl 4-(1-cyano-2-(4′-cyanobiphenyl-4-yl)ethylcarbamoyl)tetrahydro-2H-pyran-4-ylcarbamate (produced in step (iii), 5 g) was added formic acid (6 rel. vol.) at room temperature and the mixture heated to 40° C. The reaction mixture was stirred for 1.5 h at 40° C. and then cooled to 0-8° C. and quenched with water (5 rel. vol.). The reaction mixture was diluted with 2-methyltetrahydrofuran (10 rel. vol.) and 2N NaOH solution added dropwise at 0-8° C. until the pH reached 6.7. The reaction mixture was further diluted with 2-2-methyltetrahydrofuran (10 rel. vol.) and extracted. The organic layer was separated and concentrated to 8 rel. vol. under vacuum. The mixture was stirred the concentrated for 1 h at room temperature and the resulting solid was filtered and washed with 2-methyltetrahydrofuram (1 rel. vol.) to afford the titled compound (2.0 g).

1. temperaturecooled to 0-8° C.
2. customquenched with water (5 rel. vol.)
3. additionThe reaction mixture was diluted with 2-methyltetrahydrofuran (10 rel. vol.) and 2N NaOH solution
4. additionadded dropwise at 0-8° C. until the pH
5. additionThe reaction mixture was further diluted with 2-2-methyltetrahydrofuran (10 rel. vol.)
6. extractionextracted
7. customThe organic layer was separated
8. concentrationconcentrated to 8 rel
9. stirringThe mixture was stirred the
10. concentrationconcentrated for 1 h at room temperature
11. filtrationthe resulting solid was filtered
12. washwashed with 2-methyltetrahydrofuram (1 rel. vol.)