反応 #63654

ord-3b5a885978f046769cdc4f35aae7fc3f

反応条件

温度
30°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    その他was brought to 40° C.
  3. 3
    workup.STIRRINGunder stirring for seven days
  4. 4
    ろ過the unreacted carnitine chloride was filtered off
  5. 5
    workup.ADDITIONUpon addition of tert-butyl methyl ether an oil
  6. 6
    その他precipitated
  7. 7
    その他The oil precipitation
  8. 8
    その他The oil which finally separated

実験手順

A mixture of methoxyacetic acid (3 ml; 0.04 moles) and methoxyacetyl chloride (3 ml; 0.03 moles) was kept under stirring at 30° C. for 2 hours. To this mixture carnitine chloride (4 g; 0.02 moles) which had been previously dried was added. The resulting mixture was brought to 40° C. and kept under stirring for seven days. The mixture was then taken up with acetonitrile and the unreacted carnitine chloride was filtered off. Upon addition of tert-butyl methyl ether an oil precipitated. The oil precipitation was repeated four times with acetonitrile/tert butyl methyl ether. The oil which finally separated was lyophilized. Four grams of methoxy acetyl carnitine chloride were thus obtained. Yield: 75%

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04766222uspto-grants-1988_08