HRID1711418
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 mixture of 4-[3-(1-naphthylsulfonyl)-1H-indazol-5-yloxymethyl]-piperidine-1-carboxylic acid benzyl ester (0.3 g, 0.54 mmoles) and 33 wt % HBr in acetic acid (1.5 mL) was stirred at room temperature for 30 minutes, diluted with ethyl ether and filtered. The filtercake was washed with ether, dried, treated with 1N NaOH and saturated NaCl and extracted with EtOAc. The extracts were combined, dried over Na2SO4 and concentrated under vacuum to afford the title compound as an off-white solid; mp 175-177° C., identified by HNMR and mass spectral analyses, MS (ES) m/z 420.2.
WORKUP
后处理
- filtrationfiltered
- washThe filtercake was washed with ether
- customdried
- additiontreated with 1N NaOH and saturated NaCl
- extractionextracted with EtOAc
- dry with materialdried over Na2SO4
- concentrationconcentrated under vacuum