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Sulfuric acid magnesium salt (1:1) → Fingolimod Impurity 4

HRID 842265
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HRID 842265 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([NH:10][CH:11]([CH2:16][CH2:17][C:18]1[CH:23]=[CH:22][C:21]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])=[CH:20][CH:19]=1)[C:12](OC)=[O:13])(=[O:9])[CH3:8].S([O-])([O-])(=O)=O.[Mg+2]>O1CCCC1>[C:7]([NH:10][CH:11]([CH2:16][CH2:17][C:18]1[CH:23]=[CH:22][C:21]([CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])=[CH:20][CH:19]=1)[CH2:12][OH:13])(=[O:9])[CH3:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 21226445Aluminium lithium hydrideHCID 22618836Methyl 2-acetamido-4-(4-octylphenyl)butyrate

생성물 1

HCID 22618882Fingolimod Impurity 4수율 65.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

To a suspension of lithium aluminum hydride (1.2 g) in tetrahydrofuran (100 ml), a solution of methyl 2-acetamido-4-(4-octylphenyl)butyrate (11 g) in tetrahydrofuran (200 ml) was added and the suspension was stirred at room temperature for 30 minutes. An aqueous tetrahydrofuran (70%, 10 ml) was added to the solution and the mixture was left standing overnight. Magnesium sulfate was added to the mixture, the precipitate was filtered off and the solvent was distilled away under reduced pressure. The residue was dissolved in ethyl acetate, the solution was washed with a dilute hydrochloric acid, an aqueous sodium hydrogencarbonate solution and a saturated brine in order and dried over sodium sulfate. The solvent was distilled away under reduced pressure to give the subject compound (6.6 g).

후처리

  1. waitthe mixture was left
  2. waitstanding overnight
  3. filtrationthe precipitate was filtered off
  4. distillationthe solvent was distilled away under reduced pressure
  5. dissolutionThe residue was dissolved in ethyl acetate
  6. washthe solution was washed with a dilute hydrochloric acid
  7. dry with materialan aqueous sodium hydrogencarbonate solution and a saturated brine in order and dried over sodium sulfate
  8. distillationThe solvent was distilled away under reduced pressure

출처 및 근거

ORD 기록
ord-b16dbc5134e44821b961cd3a794d0875
출처 데이터셋
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06372800B1

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