HRID1160313

反应详情

EQUATION

反应方程式

HRID 1160313 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 45.3 (56 mg, 0.1 mmol) and 2N NaOH(aq) solution (0.31 mL, 0.62 mmol) in THF (3 mL) was stirred at room temperature overnight. The reactor mixture was concentrated, treated with dilute HCl, and extracted into ethyl acetate. The organic layer washed with water and concentrated to yield product which was purified by flash chromatography to give compound 45 (40 mg). 1H NMR (500 MHz, CDCl3, ppm), δ 0.9 (t, 3H), 1.4 (m, 2H), 1.65 (m, 2H), 2.35 (s, 3H), 3.05 (m, 2H), 3.9 (t, 2H), 4.5 (t, 1H), 5.05 (s, 2H), 6.8-7.5 (m, 15H). MS ESI (neg.) m/e: 511.0 (M−H).

WORKUP

后处理

  1. concentrationThe reactor mixture was concentrated
  2. additiontreated with dilute HCl
  3. extractionextracted into ethyl acetate
  4. washThe organic layer washed with water
  5. concentrationconcentrated
  6. customto yield product which
  7. customwas purified by flash chromatography