HRID2306466

反应详情

EQUATION

反应方程式

HRID 2306466 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

0.5 ml of oxalyl chloride is added to a solution of 1.2 g of 11-acetylamino-undecanoic acid and 5 drops of DMF in 15 ml of methylene chloride at 0° C. and the mixture is stirred at RT for 3 hrs. The solution of the 11-acetylamino-undecanoyl chloride is treated under argon with 0.6 g of 2-fluoroanisole, cooled to −15° C. and treated with 1.4 g of aluminium chloride. After 2 hrs. at −15° C. the mixture is left to warm to room temperature overnight. The solution is treated with 15 ml of 1M hydrochloric acid at 0° C. and then with 20 ml of water. The organic phase is separated and washed with 1M hydrochloric acid, with water and with saturated sodium bicarbonate solution, dried and concentrated. 1.8 g of N-[11-(3-fluoro-4-methoxy-phenyl)-11-oxo-undecyl]acetamide are obtained.

WORKUP

后处理

  1. temperaturecooled to −15° C.
  2. waitAfter 2 hrs
  3. waitat −15° C. the mixture is left
  4. temperatureto warm to room temperature overnight
  5. customThe organic phase is separated
  6. washwashed with 1M hydrochloric acid, with water and with saturated sodium bicarbonate solution
  7. customdried
  8. concentrationconcentrated