反应 #1483150

ord-a1db51fa70ba459898c2094c8eb17292

反应方程式

CCOC(=O)C(NC(=O)OCc1ccccc1)C(=O)OCC
diethyl 2-benzyloxycarbonylaminomalonate
O=C([O-])[O-].[K+].[K+]
potassium carbonate
[I-].[K+]
potassium iodide
CCOC(=O)CCl
ethyl 2-chloroacetate
Cl
hydrochloric acid
CCOC(=O)CC(NC(=O)OCc1ccccc1)(C(=O)OCC)C(=O)OCC
title compound
收率 86.1%
CCOC(=O)CC(NC(=O)OCc1ccccc1)(C(=O)OCC)C(=O)OCC
diethyl 2-benzyloxycarbonylamino-2-ethoxycarbonylsuccinate
收率 86.1%

溶剂

反应条件

温度
50°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction mixture was cooled
  2. 2
    萃取the mixture was extracted with ethyl acetate
  3. 3
    洗涤the extract was washed with saturated brine
  4. 4
    干燥dried over anhydrous magnesium sulfate
  5. 5
    其他The solvent was evaporated under reduced pressure
  6. 6
    其他the residue was crystallized from ethyl acetate/n-hexane

实验过程

A suspension of diethyl 2-benzyloxycarbonylaminomalonate (5.0 g), potassium carbonate (2.7 g), potassium iodide (0.27 g), and ethyl 2-chloroacetate (2.6 g) in DMF (50 mL) was stirred at 50° C. for 1 hour. The reaction mixture was cooled, and then poured into diluted hydrochloric acid, the mixture was extracted with ethyl acetate, and the extract was washed with saturated brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was crystallized from ethyl acetate/n-hexane to obtain the title compound (5.5 g, yield: 86%) as colorless crystals.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08900830B2uspto-grants-2014_12