Reaktionsgleichung
[H-].[Na+].[Cl:3][C:4]1[CH:22]=[CH:21][CH:20]=[C:19]([Cl:23])[C:5]=1[C:6]([C:8]1[C:13]([CH3:14])=[CH:12][C:11]([O:15][CH3:16])=[C:10]([OH:17])[C:9]=1[OH:18])=[O:7].I[CH2:25][CH2:26][CH2:27][CH3:28]>O1CCCC1>[CH2:25]([O:18][C:9]1[C:10]([O:17][CH2:22][CH2:4][CH2:5][CH3:6])=[C:11]([O:15][CH3:16])[CH:12]=[C:13]([CH3:14])[C:8]=1[C:6](=[O:7])[C:5]1[C:4]([Cl:3])=[CH:22][CH:21]=[CH:20][C:19]=1[Cl:23])[CH2:26][CH2:27][CH3:28]Komponenten
5
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
Sodiumhydride (0.4 g; 60%; 10 mmol) is added with stirring to a solution of 2,6-dichloro-2',3'-dihydroxy-4'-methoxy-6'-methyl-benzophenone (1.64 g; 5 mmol) in tetrahydrofurane. The solvent is evaporated and the residue dissolved in 30 ml of dimethylformamide. 1-iodo-n-butane (4.6 g; 25 mmol) is added, the mixture is stirred at 100° C. for 8 hours and then the solvent is evaporated. The residue is shaken with toluene/2N hydrochloric acid, the organic layer separated, washed with water and the solvent evaporated. The residue is purified by chromatography (flash column filled with 35 g of silicagel; elution with 500 ml of petrolether containing 2% of ethylacetate); yellow oil (0.7 g; 32% y).
Aufarbeitung
- customThe solvent is evaporated
- dissolutionthe residue dissolved in 30 ml of dimethylformamide
- customthe solvent is evaporated
- stirringThe residue is shaken with toluene/2N hydrochloric acid
- customthe organic layer separated
- washwashed with water
- customthe solvent evaporated
- customThe residue is purified by chromatography (flash column filled with 35 g of silicagel; elution with 500 ml of petrolether containing 2% of ethylacetate)
Quellen und Nachweise
- ORD-Eintrag
- ord-1c3f43f7342345d3bbb71eabe79c1ab1
- Quelldatensatz
- uspto-grants-1998_06
- Patentnummer
- US05773663
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