HRID966535
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
To a solution of 5-(tert-butoxycarbonylamino-methyl)-2-methyl-1H-indole-3-carboxylic acid benzyl ester (1.8 g, 4.6 mmol) in methylene chloride (10 μL) was added 4 M hydrogen chloride in dioxane (1.2 mL, 4.8 mmol). The mixture was stirred at room temperature for 1 hour and the formed solid was then filtered. The product was further purified by recrystallization (ethanol and methylene chloride) to give 950 mg (63%) of titled product as a beige solid: mp 260-261° C.; MS(APCI−): m/z 293.1 (M−H); Anal. Calcd for C18H18N2O2.1.06HCl: C, 64.92; H, 5.77; N, 8.41; Cl, 11.29. Found: C, 64.58; H, 5.79; N, 8.31; Cl, 11.38.
WORKUP
后处理
- filtrationthe formed solid was then filtered
- customThe product was further purified by recrystallization (ethanol and methylene chloride)