HRID28578
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 tert-butoxycarbonylamino-acetic acid 4-[2-amino-6-(5-chloro-2-ethoxy-phenyl)-pyrimidin-4-ylamino]-benzyl ester in ethyl acetate (15 ml) was treated with a solution of hydrogen chloride in dioxane (4.0 M, 15 ml). After stirring for 16 hours, the solid was filtered and dried under reduced pressure to provide the hydrochloride salt of the title compound (0.273 g, 48% yield). 1H NMR (DMSO-d6) δ 1.39 (t, 3H, J=6.4 Hz, CH3), 3.89 (d, 2H, J=4.9 Hz, CH2), 4.17 (q, 2H, J=6.2 Hz, CH2), 5.25 (s, 2H, CH2), 6.70 (s, 1H, Ar), 7.28 (d, 1H, J=8.7 Hz, Ar), 7.46 (d, 2H, J=8.4 Hz, Ar), 7.62-7.67 (m, 2H, Ar), 7.88 (d, 2H, J=7.4 Hz, Ar), 8.37 (s, 3H), 11.10 (s, 1H), 12.68 (s, 1H).
WORKUP
后处理
- filtrationthe solid was filtered
- customdried under reduced pressure