反应详情

温度

100 °C

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).

1. customThe solvent is evaporated
2. dissolutionthe residue dissolved in 30 ml of dimethylformamide
3. customthe solvent is evaporated
4. stirringThe residue is shaken with toluene/2N hydrochloric acid
5. customthe organic layer separated
6. washwashed with water
7. customthe solvent evaporated
8. customThe residue is purified by chromatography (flash column filled with 35 g of silicagel; elution with 500 ml of petrolether containing 2% of ethylacetate)