تفاعل #46264

معادلة التفاعل

2-butoxy-2-oxoethanaminium chloride

triethylamine

diethyl oxalate

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title material

Butyl N-[ethoxy(oxo)acetyl]glycinate

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe product mixture was cooled
2. 2
   تركيزconcentrated under vacuum
3. 3
   workup.DISSOLUTIONThe residue was dissolved in methylene chloride
4. 4
   غسيلwashed with two 4 L portions of water
5. 5
   تجفيفThe organic fraction was dried over anhydrous magnesium sulfate
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated under vacuum
8. 8
   أخرىCollection and concentration of appropriate fractions

الإجراء التجريبي

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.

المصدر