4-(2-甲氧基乙氧基)-3-氧代丁酸乙酯

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Ethyl 4-(2-methoxyethoxy)-3-oxobutanoate (Intermediate 123) (0.5 g) was dissolved in anhydrous DCM (5 ml). Sulfuryl chloride (430 mg) was added dropwise at room temperature. The mixture was stirred for 6 h. The crude mixture was diluted with EtOAc (50 ml) and washed well with water and brine, dried over sodium sulfate and concentrated in vacuo to afford the title compound as a light orange oil (414 mg). washed well with water and brine dried over sodium sulfate concentrated in vacuo

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2,2-Dimethyl-1,3-dioxane-4,6-dione (1.72 g) was suspended in anhydrous pyridine (20 ml) and cooled to 0° C. (2-methoxyethoxy)acetyl chloride (2 g) was added slowly. The mixture was stirred at room temperature for 3 h. The mixture was poured into 2 N HCl (30 ml) and extracted with DCM (×3). The combined organic phase was washed with water, brine, dried over sodium sulfate and concentrated in vacuo. The orange oil was dissolved in EtOH (20 ml) and was refluxed for 7 h. The solvent was removed in vacuo and the brown oil was Kugelrohr distilled affording the title compound as a colourless oil (1.55 g). was added slowly extracted with DCM (×3) The combined organic phase was washed with water, brine dried over sodium sulfate concentrated in vacuo The orange oil was dissolved in EtOH (20 ml) was refluxed for 7 h The solvent was removed in vacuo distilled

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 2,2-Dimethyl-1,3-dioxane-4,6-dione (1.72 g) was suspended in anhydrous pyridine (20 ml) and cooled to 0° C. (2-methoxyethoxy)acetyl chloride (2 g) was added slowly. The mixture was stirred at room temperature for 3 h. The mixture was poured into 2 N HCl (30 ml) and extracted with DCM (×3). The combined organic phase was washed with water, brine, dried over sodium sulfate and concentrated in vacuo. The orange oil was dissolved in EtOH (20 ml) and was refluxed for 7 h. The solvent was removed in vacuo and the brown oil was Kugelrohr distilled affording the title compound as a colourless oil (1.55 g). was added slowly extracted with DCM (×3) The combined organic phase was washed with water, brine dried over sodium sulfate concentrated in vacuo The orange oil was dissolved in EtOH (20 ml) was refluxed for 7 h The solvent was removed in vacuo distilled