HRID1244024

反应详情

EQUATION

反应方程式

HRID 1244024 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under nitrogen, combined 1.0 g of imidazole (14.7 mmol) with 824 mg of potassium hydroxide (14.7 mmol), 2.0 g of potassium carbonate (14.7 mmol) and 82 mg of benzyltriethylammonium chloride (7.34 mmol) in 40 ml of CH2Cl2. Added 695 μl of methylbromoacetate. Reaction is stirred at room temperature for 3 hours. Filtered off solids, rinsed with CH2Cl2, and evaporated the filtrate under reduced pressure to give colorless oil. Product is purified by flash chromatography on a Biotage Flash 40 (Eluent: 95:5 CH2Cl2/CH3OH), yielding 300 mg of a white solid (27%). 1H NMR (400 MHz, CD3OD) δ 3.75 (3H, s), 4.91 (2H, s), 6.96 (1H, s), 7.10 (1H, s), 7.64 (1H, s).

WORKUP

后处理

  1. customReaction
  2. filtrationFiltered off solids
  3. washrinsed with CH2Cl2
  4. customevaporated the filtrate under reduced pressure
  5. customto give colorless oil
  6. customProduct is purified by flash chromatography on a Biotage Flash 40 (Eluent: 95:5 CH2Cl2/CH3OH)