Реакция #46264

Уравнение реакции

2-butoxy-2-oxoethanaminium chloride

triethylamine

diethyl oxalate

→

title material

Butyl N-[ethoxy(oxo)acetyl]glycinate

Растворители

ethanol

Условия реакции

Обработка

1. 1
   ТемператураThe product mixture was cooled
2. 2
   Концентрированиеconcentrated under vacuum
3. 3
   workup.DISSOLUTIONThe residue was dissolved in methylene chloride
4. 4
   Промывкаwashed with two 4 L portions of water
5. 5
   СушкаThe organic fraction was dried over anhydrous magnesium sulfate
6. 6
   Фильтрацияfiltered
7. 7
   Концентрированиеconcentrated under vacuum
8. 8
   ДругоеCollection and concentration of appropriate fractions

Методика

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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