반응 #63655

반응 방정식

carnitine

ethoxyacetyl chloride

ethoxy acetic acid

ethoxyacetyl chloride

carnitine chloride

→

title compound

수율 75.0%

ethoxy acetyl carnitine chloride

수율 75.0%

용매

tert-butyl methyl ether

반응 조건

후처리

1. 1
   기타had been prepared
2. 2
   workup.ADDITIONwas added
3. 3
   workup.WAITat 40° C. for eight days
4. 4
   workup.WAITthe resulting mixture was kept at 40° C. for seven days
5. 5
   workup.ADDITIONUpon addition
6. 6
   기타precipitated
7. 7
   기타The oil precipitation
8. 8
   기타until complete removal of the ethoxyacetic acid in excess

실험 절차

A mixture of ethoxy acetic acid (5 ml; 0.07 moles) and ethoxyacetyl chloride (1.8 ml; 0.015 moles) which had been prepared as disclosed in step (b) of Example 5, was kept under stirring for 2 hours at 80° C. To this mixture carnitine chloride (2 g; 0.01 moles) which had been previously dried was added. The resulting mixture was first kept at 80° C. until complete dissolution of carnitine took place, then at 40° C. for eight days. A further amount of ethoxyacetyl chloride (0.9 ml; 0.007 moles) was added and the resulting mixture was kept at 40° C. for seven days. Upon addition to the mixture of tert-butyl methyl ether an oil precipitated. The oil precipitation was repeated four times with acetonitrile/tert butyl methyl ether until complete removal of the ethoxyacetic acid in excess. 1.5 grams of the title compound were thus obtained. Yield: 75%

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