反应详情

Preparation of N—((S)-1-((3R,3aR,6aR)-3-Hydroxydihydro-2H-furo[3,2-b]pyrrol-4(5H, 6H,6aH)-yl)-4-methyl-1-oxopentan-2-yl)-4-(4-propylpiperazin-1-yl)benzamide A solution of HCl in 1,4-dioxane (4.0M, 22 mL, 88 mmol) was added to tert-butyl(S)-1-((3R,3aR,6aR)-3-hydroxydihydro-2H-furo[3,2-b]pyrrol-4(5H,6H,6aH)-yl)-4-methyl-1-oxopentan-2-ylcarbamate (1.335 g, 3.90 mmol). The solution was stirred for 2.5 hours then the solvents were removed in vacuo and the residue azeotroped with toluene (3×30 mL) to leave (S)-2-amino-1-((3R,3aR,6aR)-3-hydroxydihydro-2H-furo[3,2-b]pyrrol-4(5H,6H,6aH)-yl)-4-methylpentan-1-one hydrochloride as an off-white solid which was used without further purification. TLC (Rf=0.0, EtOAc:heptane 3:1), analytical HPLC main peak, Rt=3.54 min., HPLC-MS 243.2 [M+H]+, 507.3 [2M+Na]+.

1. customthe solvents were removed in vacuo
2. customthe residue azeotroped with toluene (3×30 mL)