HRID1358752

反应详情

EQUATION

反应方程式

HRID 1358752 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. extractionextracted with EtOAc
  2. washwashed with organic layer with water, brine
  3. customdried
  4. concentrationconcentrated
  5. customchromatographed to give{4-[4-(4-trifluoromethanesulfonyl-phenoxy)-benzenesulfonyl]-phenoxy}-acetic acid ethyl ester