HRID1067859

反应详情

EQUATION

反应方程式

HRID 1067859 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(4-[2-(6,11-Dihydrodibenzo[b,e]thiepin-11-yloxy)-ethoxy]-phenyl)-2-ethoxy-propionic acid ethyl ester (example 2) (220 mg, 0.44 mmol) in ethanol (5 mL) was added NaOH 1 N (0.9 mL, 0.9 mmol). The mixture was stirred at room temperature for 16 h. The ethanol was evaporated of and pH adjusted with HCl 1 N to pH 1. After extraction with dichloromethane the product was purified by chromatography, using dichloromethane/methanol (9:1) as eluent, to give 126 mg (62%) of the title compound: 1H NMR (300 MHz, CDCl3) δ1.15 (t, 3H), 2.85-3.10 (m, 2H), 3.32-3.42 (m, 1H), 3.52-3.65 (m, 1H), 2.85 (t, 2H), 3.95-4.05 (m, 1H), 4.10-4.22 (m, 2H), 4.5-5.1 (bs, 1H), 5.60-5.75 (bs, 1H), 6.82 (d, 2H), 7.05-7.50 (m, 10H).

WORKUP

后处理

  1. customThe ethanol was evaporated of and
  2. extractionAfter extraction with dichloromethane the product
  3. customwas purified by chromatography