1,2-Dimethoxyethane → HCID 54517826, Verbindung

HRID 1031507

Reaktionsgleichung

Reaktionsgleichung von HRID 1031507
C(OP(CC([N:12]1[CH2:17][CH2:16][O:15][CH2:14][CH2:13]1)=O)(OCC)=O)C.C[C:19]([CH3:22])([O-:21])C.[K+].[Cl:24][C:25]1[CH:49]=[CH:48][C:28]([O:29][C:30]2[CH:31]=[CH:32][C:33]([C:36](=O)[C:37]3[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[C:39]([O:45][CH3:46])[CH:38]=3)=[N:34][CH:35]=2)=[CH:27][CH:26]=1.C[O:51]CCOC>>[Cl:24][C:25]1[CH:49]=[CH:48][C:28]([O:29][C:30]2[CH:31]=[CH:32][C:33]([C:36]([C:37]3[CH:42]=[CH:41][C:40]([O:43][CH3:44])=[C:39]([O:45][CH3:46])[CH:38]=3)=[CH:22][C:19]([O:51][N:12]3[CH2:13][CH2:14][O:15][CH2:16][CH2:17]3)=[O:21])=[N:34][CH:35]=2)=[CH:27][CH:26]=1

Komponenten

6

Edukt 5

HCID 80711,2-DimethoxyethaneHCID 11207805Phosphonic acid, [2-(4-morpholinyl)-2-oxoethyl]-, diethyl esterHCID 148232335-(4-Chlorophenoxy)-2-(3,4-dimethoxybenzoyl)pyridineHCID 23665647Potassium tert-butoxideHCID 178418922HCID 178418922, Verbindung

Produkt 1

HCID 54517826HCID 54517826, Verbindung

Versuchsvorschrift

In 1,2-dimethoxyethane (10 ml) was dissolved diethylphosphonoacetic acid morpholide (210 mg), to which was added 90% potassium tert-butoxide (100 mg). To the mixture was added, after the tert-butoxy potassium was completely dissolved, 5-(4-chlorophenoxy)-2-(3,4-dimethoxybenzoyl)pyridine (240 mg). The mixture was stirred for one hour at room temperature and for 6 hours at 50° C. to 60° C. The reaction mixture was concentrated, and there was added water (30 ml), followed by extraction with ethyl acetate (70 ml×2). The extract solution was dried over anhydrous magnesium sulfate, and was subjected to filtration to remove the magnesium sulfate. The filtrate was concentrated and purified by means of a silica gel column chromatography (eluted with ethyl acetate) to obtain 4-[3-(5-(4-chlorophenoxy)-2-pyridyl)-3-(3,4-dimethoxyphenyl)acryloxy]morpholine (Compound No.88) (300 mg) as a resinous solid.

Aufarbeitung

  1. additionTo the mixture was added
  2. concentrationThe reaction mixture was concentrated
  3. additionthere was added water (30 ml)
  4. extractionfollowed by extraction with ethyl acetate (70 ml×2)
  5. dry with materialThe extract solution was dried over anhydrous magnesium sulfate
  6. filtrationwas subjected to filtration
  7. customto remove the magnesium sulfate
  8. concentrationThe filtrate was concentrated
  9. custompurified by means of a silica gel column chromatography (eluted with ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-1289fb28f3824ab5b155337c9044b748
Quelldatensatz
uspto-grants-1990_09
Patentnummer
US04954497

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