HRID1923

反应详情

EQUATION

反应方程式

HRID 1923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The FMOC amide from Step F (1.15 g; 1.88 mmol) was dissolved in methylene chloride (10 ml) and 4-(aminomethyl)piperidine (1 ml) added. The reaction mixture was stirred at room temperature. The reaction mixture was stirred for 15 minutes and then quenched by adding water. The methylene chloride phase was separated, dried over ahnydrous potassium carbonate powder, filtered and evaprated under reduced pressure to afford an orange-yellow oil. The oil was chromatographed on silica gel using an eluant of ethyl acetate and methanol (9:1 v/v). A pale yellow oil (517 mg; 70.6%) was isolated of the amine. FAB-MS:- calculated for C23H23N3 O3 389.2 found 389.9 (M).

WORKUP

后处理

  1. stirringThe reaction mixture was stirred for 15 minutes
  2. customquenched
  3. additionby adding water
  4. customThe methylene chloride phase was separated
  5. dry with materialdried over ahnydrous potassium carbonate powder
  6. filtrationfiltered
  7. customto afford an orange-yellow oil
  8. customThe oil was chromatographed on silica gel using an eluant of ethyl acetate and methanol (9:1 v/v)