DL-Carnitine → Ethoxy acetyl carnitine chloride

HRID 35377

반응식

HRID 35377 반응식
[CH2:1]([O:3][CH2:4][C:5]([OH:7])=O)[CH3:2].C(OCC([Cl:14])=O)C.[CH3:15][N+:16]([CH2:19][CH:20]([OH:25])[CH2:21][C:22]([O-:24])=[O:23])([CH3:18])[CH3:17]>COC(C)(C)C>[CH2:1]([O:3][CH2:4][C:5]([C:20]([CH2:21][C:22](=[O:23])[O-:24])([CH2:19][N+:16]([CH3:15])([CH3:17])[CH3:18])[OH:25])=[O:7])[CH3:2].[Cl-:14]

참가 물질

5

반응물 3

HCID 288DL-Carnitine2회HCID 12301Ethoxyacetic acidHCID 84189Ethoxyacetyl chloride2회

생성물 1

HCID 131715706Ethoxy acetyl carnitine chloride수율 75%

시약·촉매·용매 1

HCID 15413tert-Butyl methyl ether용매

반응 조건

온도
80 °C

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%

후처리

  1. customhad been prepared
  2. additionwas added
  3. waitat 40° C. for eight days
  4. waitthe resulting mixture was kept at 40° C. for seven days
  5. additionUpon addition
  6. customprecipitated
  7. customThe oil precipitation
  8. customuntil complete removal of the ethoxyacetic acid in excess

출처 및 근거

ORD 기록
ord-f5d28144541a4d72ab9b187af1c7add8
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766222

연결된 노트

불러오는 중…