Carnitine Chloride → p-Isobutylphenyl-alpha-methyl acetyl carnitine hydrochloride

HRID 435478

반응식

HRID 435478 반응식
[CH3:1][N+:2]([CH2:5][CH:6]([OH:11])[CH2:7][C:8]([OH:10])=[O:9])([CH3:4])[CH3:3].[Cl-].[CH2:13]([C:17]1[CH:22]=[CH:21][C:20](C(C)C([Cl:26])=O)=[CH:19][CH:18]=1)[CH:14]([CH3:16])[CH3:15]>C(O)(C(F)(F)F)=O>[ClH:26].[CH2:13]([C:17]1[CH:18]=[CH:19][C:20]([CH:5]([N+:2]([CH3:3])([CH3:4])[CH3:1])[C:6]([C:8](=[O:9])[CH2:7][CH3:6])([CH2:7][C:8](=[O:10])[O-:9])[OH:11])=[CH:21][CH:22]=1)[CH:14]([CH3:16])[CH3:15]

참가 물질

4

반응물 2

HCID 5970Carnitine ChlorideHCID 595157alpha-Methyl-4-(2-methylpropyl)benzeneacetyl chloride

생성물 1

HCID 131713075p-Isobutylphenyl-alpha-methyl acetyl carnitine hydrochloride수율 65%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

4.95 g (0.025 moles) of D,L-carnitine hydrochloride are dissolved in 8 mls of CF3COOH, and to the solution an excess (16 mls) of p-isobutylphenyl-alpha-methyl acetyl chloride is added and the mixture is kept under stirring at a temperature of 40°-45° C. for 4-5 hours. At the end of this period of time, the mixture is partitioned with H2O--CHCl3, the organic phase is discarded whereas the aqueous phase is concentrated under reduced pressure at a bath temperature of about 50° C. A gelatinous raw material is obtained which is crystallized with isopropanol. The precipitate thus obtained is filtered, rapidly washed with ether because of its hydroscopicity, and dried under vacuum at a temperature not exceeding 50° C.; 6.3 g of a product are obtained (yield 65%) having the following characteristics:

후처리

  1. customAt the end of this period of time, the mixture is partitioned with H2O--CHCl3
  2. concentrationis concentrated under reduced pressure at a bath temperature of about 50° C
  3. customA gelatinous raw material is obtained which
  4. customis crystallized with isopropanol
  5. customThe precipitate thus obtained
  6. filtrationis filtered
  7. washrapidly washed with ether because of its hydroscopicity
  8. customdried under vacuum at a temperature not
  9. customexceeding 50° C.

출처 및 근거

ORD 기록
ord-76ef5ee9ab87465a92aad006b091e810
출처 데이터셋
uspto-grants-1983_08
특허 번호
US04401827

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