HRID33748

反应详情

EQUATION

反应方程式

HRID 33748 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

[4-(4-Isopropyl-piperazine-1-carbonyl)-oxazol-2-ylmethyl]-(2-methoxy-ethyl)-carbamic acid tert-butyl ester. A mixture of the crude material from Step C (1.10 g, 3.67 mmol), 1-isopropyl-piperazine dihydrochloride (0.810 g, 4.03 mmol), 1-hydroxybenzotriazole (0.595 g, 4.40 mmol), and N-methylmorpholine (2.42 mL, 22.0 mmol) in DMF (20 mL) was stirred for 1 h. 1-(3-Dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.845 g, 4.40 mmol) was added and the mixture was stirred overnight. The reaction mixture was diluted with H2O (500 mL) and extracted with DCM (3×60 mL). The combined organic extracts were washed with H2O (3×300 mL), dried over Na2SO4, filtered and concentrated to yield the crude title compound (1.30 g). MS (ESI): exact mass calcd. for C20H34N4O5, 410.25; m/z found, 411.5 [M+H]+.

WORKUP

后处理

  1. stirringthe mixture was stirred overnight
  2. extractionextracted with DCM (3×60 mL)
  3. washThe combined organic extracts were washed with H2O (3×300 mL)
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated