HRID913246
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
A solution of pyridin-3-ylmethyl {4-[({4-[(tert-butoxycarbonyl)amino]-1-phenyl-1H-pyrazol-3-yl}amino)carbonyl]benzyl}carbamate (0.075 g, 0.14 mmol) in ethyl acetate (2 mL) and methanol (1 mL) was treated with 4M HCl in dioxane (3.11 mL, 12.4 mmol) and stirred at ambient temperature for 12 hours. The reaction was evaporated in vacuo and purified by flash column chromatography (0-5% methanol/methylene chloride w/0.1% ammonia) to give the title compound as an off-white solid. 1H NMR (CD3OD) δ 8.58 (s, 1H), 8.48 (m, 1H), 7.96 (d, J=8.22 Hz, 2H), 7.87 (d, J=8.22 Hz, 1H), 7.79 (s, 1H), 7.65 (d, J=8.22 Hz, 2H), 7.42 (m, 5H), 7.22 (t, J=7.30 Hz, 1H), 5.18 (s, 2H), 4.38 (s, 2H).
WORKUP
后处理
- customThe reaction was evaporated in vacuo
- custompurified by flash column chromatography (0-5% methanol/methylene chloride w/0.1% ammonia)