HRID1040459

反应详情

EQUATION

反应方程式

HRID 1040459 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To (S)-2-tert-Butoxycarbonylamino-propionic acid (1.54 g, 8.12 mmol), Amino-pyridin-2-yl-acetic acid methyl ester (1.35 g, 8.12 mmol) and HATU (3.1 g, 8.12 mmol) was added the DMF (20 mL) and Et3N (2.26 ml, 16.20 mmol) and the solution was stirred for 2 h. The mixture was concentrated to remove most of the DMF was removed. The resulting oil was dissolved in EtOAc, washed with water, 0.1 N HCl aq., 1 N NaHCO3 aq., followed by Brine. The combined organics were dried over MgSO4, filtered, and concentrated in vacuo to provide ((S)-2-tert-Butoxycarbonylamino-propionylamino)-pyridin-2-yl-acetic acid methyl ester (2.7 g, 98%) as a yellow oil, m/z 338.61 [M+1]+

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. customto remove most of the DMF
  3. customwas removed
  4. dissolutionThe resulting oil was dissolved in EtOAc
  5. washwashed with water, 0.1 N HCl aq., 1 N NaHCO3 aq.
  6. dry with materialThe combined organics were dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo