HRID725273

反应详情

EQUATION

反应方程式

HRID 725273 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 303 mg (2.1 mmol) of 2-naphthol in 5 mL of dry ether was treated with 50 mg (2.1 mmol) of sodium hydride and the mixture was stirred for 15 minutes. A solution of 368 mg (1.0 mmol) of the compound of step C in 5 mL of dry ether and 126 mg (0.174 mL, 1.22 mmol) of triethylamine was cooled to 0° C. and treated with 114 mg (0.077 mL, 1.0 mmol) of methanesulfonyl chloride. Triethylamine hydrochloride was removed by filtration and the filtrate was added to the above suspension of sodium 2-naphthoxide and the reaction mixture was stirred at room temperature for 12 hours. The reaction mixture was then partitioned between water and ether and the organic extracts were dried and evaporated to give the desired product in 29% yield. 1H-NMR (CDCl3) δ1.00 (3H, t, J=7), 1.20 (3H, t, J=7), 2.44 (2H, q, J=7), 4.58 (2H, s), 6.96-7.84 (8H, m).

WORKUP

后处理

  1. customTriethylamine hydrochloride was removed by filtration
  2. additionthe filtrate was added to the above suspension of sodium 2-naphthoxide
  3. stirringthe reaction mixture was stirred at room temperature for 12 hours
  4. customThe reaction mixture was then partitioned between water and ether
  5. customthe organic extracts were dried
  6. customevaporated