反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Trifluoroacetic acid (1 mL, 12.98 mmol) was added to a solution of (3 aS,4R,5R,6aS)-tert-butyl 5-(6-bromo-3-carbamoylpyrrolo[1,2-b]pyridazin-4-ylamino)-4-methylhexahydrocyclopenta[c]pyrrole-2(1H)-carboxylate (250 mg, 0.523 mmol) in dichloromethane (2 mL). After stirring for 1 h at room temperature, the mixture was concentrated and dried under high vacuum to give 6-bromo-4-(((3aS,4R,5R,6aS)-4-methyloctahydrocyclopenta[c]pyrrol-5-yl)amino)pyrrolo[1,2-b]pyridazine-3-carboxamide TFA salt (255 mg). 1H NMR (400 MHz, methanol-d4) δ ppm 8.15 (1 H, s), 7.66 (1 H, d, J=1.54 Hz), 7.06 (1 H, d, J=1.54 Hz), 4.03-4.34 (1 H, m), 3.31-3.59 (3 H, m), 3.01-3.25 (2 H, m), 2.53-2.83 (2 H, m), 1.60-1.84 (1 H, m), 1.36-1.60 (1 H, m), 1.17 (3 H, d); MS (ES+) m/z: 378.1, 380.1 (M+H).
WORKUP
后处理
- concentrationthe mixture was concentrated
- customdried under high vacuum