HRID2262508

反应详情

EQUATION

反应方程式

HRID 2262508 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3-(4-Phenyl-piperazine-1-carbonyloxymethyl)-morpholine-4-carboxylic acid tert-butyl ester (3.31 g, 8.16 mmol) was stirred in DCM (30 mL) at 0° C. TFA (6 mL) dissolved in DCM (24 mL) was added dropwise. The reaction mixture was stirred overnight at room temperature. The solvents were removed in vacuo and the residue was partitioned between DCM (30 mL) and aq NaHCO3 (5 g in 30 mL). The aqueous layer was extracted with DCM (3×30 mL), dried (MgSO4) and the solvents were removed in vacuo to give morpholin-3-ylmethyl 4-phenylpiperazine-1-carboxylate (2.55 g, quant.) as a white solid.

WORKUP

后处理

  1. additionwas added dropwise
  2. customThe solvents were removed in vacuo
  3. customthe residue was partitioned between DCM (30 mL) and aq NaHCO3 (5 g in 30 mL)
  4. extractionThe aqueous layer was extracted with DCM (3×30 mL)
  5. dry with materialdried (MgSO4)
  6. customthe solvents were removed in vacuo