反应详情

温度

50 °C

Charge 670 mL of 5 M hydrochloric acid (3.35 mol) to a solution of tert-butyl 2-(2,3-dihydro-1H-inden-2-ylamino)-5,7-dihydro-6H pyrrolo[3,4-d]pyrimidine-6-carboxylate (226 g, 641.25 mmol) in tetrahydrofuran (2.0 L) at 17° C., maintaining the internal temperature below 26° C. during the addition. Heat the resulting solution to 50° C. for 16 h, cool to 25° C. and dilute with 500 mL of water and 500 mL of tert-butylmethylether. Separate the resulting layers and extract with tert-butylmethylether (3×1 L). Concentrate the water phase down to a reaction volume of ca. 200 mL, and filter the resulting slurry. Rinse the cake with tert-butylmethylether (2×200 mL) and dry to give the title product (177 g, 80%) as a light brown solid. MS (m/z): 253.2 (M−2HCl—H2O+1).

1. temperaturemaintaining the internal temperature below 26° C.
2. additionduring the addition
3. temperaturecool to 25° C.
4. customSeparate the resulting layers
5. extractionextract with tert-butylmethylether (3×1 L)
6. concentrationConcentrate the water phase down to a reaction volume of ca. 200 mL
7. filtrationfilter the resulting slurry
8. washRinse the cake with tert-butylmethylether (2×200 mL)
9. customdry