HRID1096625

反应详情

EQUATION

反应方程式

HRID 1096625 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-15 °C

PROCEDURE

实验过程

Into a 25 mL round bottomed was added 1-fluoro-3-methoxy-2-nitrobenzene (500 mg, 2.92 mmol) and N,N-dimethylforamide (5.8 mL). The flask was cooled to −15° C. and 3-methoxypropylamine (313 mg, 3.5 mmol) in N,N-dimethylforamide (2.2 mL) was slowly added. The reaction was allowed to warm to room temperature overnight. Solvent was removed under vacuum and the residue was purified by column chromatography (20% ethylacetate:hexanes) to give 3-methoxy-N-(3-methoxypropyl)-2-nitroaniline (37A) as a yellow oil (560 mg, 80% yield). ESI-MS:m/z 241.3 (M+H)+.

WORKUP

后处理

  1. temperatureto warm to room temperature overnight
  2. customSolvent was removed under vacuum
  3. customthe residue was purified by column chromatography (20% ethylacetate:hexanes)