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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of ethyl [4-(4-hydroxyphenylsulfonyl)phenoxy]acetate (100 mg, 0.3 mmol), 4-(trifluoromethylsulfonyl)chlorobenzene (73 mg, 1 equiv.) and potassium carbonate (164 mg, 4 equiv.) in DMF was heated to 100° C. overnight. The reaction was poured into water, extracted with EtOAc, washed with organic layer with water, brine, dried and concentrated. The residue was column chromatographed to give{4-[4-(4-trifluoromethanesulfonyl-phenoxy)-benzenesulfonyl]-phenoxy}-acetic acid ethyl ester. 1HNMR (300 MHz, DMSO-d6) δ 8.11 (d, J=8.92 Hz, 2H), 8.03 (d, J=8.77 Hz, 2H), 7.90 (d, J=8.98 Hz, 2H), 7.39-7.43 (m, 4H), 7.14 (d, J=8.77 Hz, 2H), 4.90 (s, 2H, CH2), 4.15 (q, J=7.02 Hz, 2H, OCH2CH3), 1.19 (t, J=7.02 Hz, 3H, OCH2CH3). MS-EI m/z 544 [M+].
WORKUP
后处理
- extractionextracted with EtOAc
- washwashed with organic layer with water, brine
- customdried
- concentrationconcentrated
- customchromatographed to give{4-[4-(4-trifluoromethanesulfonyl-phenoxy)-benzenesulfonyl]-phenoxy}-acetic acid ethyl ester