HRID1168622
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 suspension of title B compound (213 mg, 1.30 mmol) in THF (6 mL) was added triethylamine 0.42 mL, 3.0 mmol). After stirring for 5 minutes, 4-hexyloxybenzoyl chloride (0.223 mL, 1.00 mmol) was added. After stirring for 4 hours, the reaction was filtered through a Celite pad. The pad was rinsed with ether (4×5 mL) and the combined filtrates were concentrated in vacuo. Purification by RP-HPLC (YMC SH-365-10 120A S-110 30×500 mm column, 40 mL/minute, 90:10 methanol/water containing 0.1% TFA)) afforded the title compound as a 1:1 mixture of cis- and trans- isomers (43 mg). MS: (ESI) (m/z) 332.
WORKUP
后处理
- stirringAfter stirring for 4 hours
- filtrationthe reaction was filtered through a Celite pad
- washThe pad was rinsed with ether (4×5 mL)
- concentrationthe combined filtrates were concentrated in vacuo
- customPurification by RP-HPLC (YMC SH-365-10 120A S-110 30×500 mm column, 40 mL/minute, 90:10 methanol/water containing 0.1% TFA))