奥扎格雷杂质6

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

实验步骤: Preparation as in Example 2C with 362 mg (1 mmol) of 2,4-dimethyl-3-octadecanoylpyrrole (Lehr M., WO95/13266) in place of 3-dodecanoyl-2,4-dimethylpyrrole and with ethyl (E)-4-(bromomethyl)-cinnamate in place of ethyl (E)-3-(bromo-methyl)cinnamate.

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

实验步骤: 2 g (7.43 mmol) of ethyl (E)-3-(4-bromomethylphenyl)acrylate is added to a suspension of 0.69 mL (8.2 mmol) of pyrrolidine and 2.05 g (14.86 mmol) of potassium carbonate in 40 mL of DMF and stirred for 18 hours at ambient temperature. The reaction mixture is evaporated down and the residue is extracted with water and ethyl acetate. The organic phase is dried over sodium sulfate, evaporated down, and the residue is purified by column chromatography on silica gel (eluant: dichloromethane/methanol/ammonia (90:10:1)). Yield: 0.3 g (15.6% of theory); C16H21NO2 (M=259.35); calc.: molecular ion peak (M+H)+: 260; found: molecular ion peak (M+H)+: 260; Rf value: 0.5 (silica gel, dichloromethane/methanol/ammonia (90:10:1)). The reaction mixture is evaporated down the residue is extracted with water and ethyl acetate The organic phase is dried over sodium sulfate evaporated down the residue is purified by column chromatography on silica gel (eluant: dichloromethane/methanol/ammonia (90:10:1))

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

实验步骤: Preparation as in Example 2C with 362 mg (1 mmol) of 2,4-dimethyl-3-octadecanoylpyrrole (Lehr M., WO95/13266) in place of 3-dodecanoyl-2,4-dimethylpyrrole and with ethyl (E)-4-(bromomethyl)-cinnamate in place of ethyl (E)-3-(bromo-methyl)cinnamate.

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

实验步骤: Preparation as in Example 2C with 362 mg (1 mmol) of 2,4-dimethyl-3-octadecanoylpyrrole (Lehr M., WO95/13266) in place of 3-dodecanoyl-2,4-dimethylpyrrole and with ethyl (E)-4-(bromomethyl)-cinnamate in place of ethyl (E)-3-(bromo-methyl)cinnamate.

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

实验步骤: 2 g (7.43 mmol) of ethyl (E)-3-(4-bromomethylphenyl)acrylate is added to a suspension of 0.69 mL (8.2 mmol) of pyrrolidine and 2.05 g (14.86 mmol) of potassium carbonate in 40 mL of DMF and stirred for 18 hours at ambient temperature. The reaction mixture is evaporated down and the residue is extracted with water and ethyl acetate. The organic phase is dried over sodium sulfate, evaporated down, and the residue is purified by column chromatography on silica gel (eluant: dichloromethane/methanol/ammonia (90:10:1)). Yield: 0.3 g (15.6% of theory); C16H21NO2 (M=259.35); calc.: molecular ion peak (M+H)+: 260; found: molecular ion peak (M+H)+: 260; Rf value: 0.5 (silica gel, dichloromethane/methanol/ammonia (90:10:1)). The reaction mixture is evaporated down the residue is extracted with water and ethyl acetate The organic phase is dried over sodium sulfate evaporated down the residue is purified by column chromatography on silica gel (eluant: dichloromethane/methanol/ammonia (90:10:1))

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

实验步骤: Preparation as in Example 2C with 362 mg (1 mmol) of 2,4-dimethyl-3-octadecanoylpyrrole (Lehr M., WO95/13266) in place of 3-dodecanoyl-2,4-dimethylpyrrole and with ethyl (E)-4-(bromomethyl)-cinnamate in place of ethyl (E)-3-(bromo-methyl)cinnamate.