반응 #46264

반응 방정식

2-butoxy-2-oxoethanaminium chloride

triethylamine

diethyl oxalate

→

title material

Butyl N-[ethoxy(oxo)acetyl]glycinate

용매

ethanol

반응 조건

후처리

1. 1
   온도The product mixture was cooled
2. 2
   농축concentrated under vacuum
3. 3
   workup.DISSOLUTIONThe residue was dissolved in methylene chloride
4. 4
   세척washed with two 4 L portions of water
5. 5
   건조The organic fraction was dried over anhydrous magnesium sulfate
6. 6
   여과filtered
7. 7
   농축concentrated under vacuum
8. 8
   기타Collection and concentration of appropriate fractions

실험 절차

A mixture of 2-butoxy-2-oxoethanaminium chloride (573.5 g, 3.42 mol), triethylamine (415 g, 4.1 mol), and diethyl oxalate (1.0 kg, 6.8 mol) in ethanol (7 L) was heated at 50° C. for 3 hours. The product mixture was cooled and concentrated under vacuum. The residue was dissolved in methylene chloride and washed with two 4 L portions of water. The organic fraction was dried over anhydrous magnesium sulfate, filtered, and concentrated under vacuum. The residual oil was subjected to column chromatography on silica gel eluting with heptane/ethyl acetate gradient. Collection and concentration of appropriate fractions provided the title material.

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