维拉帕米杂质26

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: 21.4 g Di-sodium tetra-iodoterephthalate, 0.5 g sodium iodide, and 10 g 2-chloropropanol were heated with stirring in 150 ml dimethylformamide at 100° C for 10 hours. The solvent was distilled off, and the residue was suspended in water and purified as described in Example 1. 14.15 g Bis-1-hydroxy-2-propyl ester of tetra-iodoterephthalic acid (60% yield) was recovered. It melted and decomposed at about 225° C. The solvent was distilled off purified

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: 0.7 g of sodium acetate was added to 7.5 g of 2-chloropropanol, to which 7.4 g of diketene was added dropwise with stirring while the reaction temperature was maintained at 40°-50° C. The reaction mixture was stirred at room temperature for an additional 2 hours and then worked up in the manner described in Referential Example 4. The resulting crude product was purified by distillation to obtain 9.8 g of 2-chloropropyl acetoacetate. was added dropwise was maintained at 40°-50° C The reaction mixture was stirred at room temperature for an additional 2 hours The resulting crude product was purified by distillation

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

实验步骤: 0.7 g of sodium acetate was added to 7.5 g of 2-chloropropanol, to which 7.4 g of diketene was added dropwise with stirring while the reaction temperature was maintained at 40°-50° C. The reaction mixture was stirred at room temperature for an additional 2 hours and then worked up in the manner described in Referential Example 4. The resulting crude product was purified by distillation to obtain 9.8 g of 2-chloropropyl acetoacetate. was added dropwise was maintained at 40°-50° C The reaction mixture was stirred at room temperature for an additional 2 hours The resulting crude product was purified by distillation

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

实验步骤: A solution of isopropylmagnesium chloride [prepared by the reaction of magnesium (2.4 g) and 2-chloropropane (10 ml) in tetrahydrofuran (30 ml)] was added dropwise under argon at -20° C. to a solution of 2-chloropropan-1-ol (9.45 g) in tetrahydrofuran (100 ml). Magnesium (3.6 g) was added and the mixture was allowed to stand for twenty minutes and was then heated under relux in the presence of 1,2-dibromopropane for 40 minutes. 1-(4-Chlorophenyl)cyclobutanecarbonitrile (9 g) was added and the mixture was heated under reflux for 16 hours. The mixture was cooled and the supernatant liquid decanted from excess magnesium metal and treated with sodium borohydride (3 g) and propan-2-ol (100 ml). The mixture was heated under reflux for 5 hours. The reaction mixture was cooled, added to water and excess concentrated hydrochloric acid was added. The resulting solution was washed with toluene, basified and extracted with toluene. The extracts were dried and evaporated to give a residue which was distilled in a Buchi Kugelrohr apparatus (140°/0.4 mm) to give 4-amino-4-[1-(4-chlorophenyl)cyclobutyl]butan-1-ol. to stand for twenty minutes the mixture was heated under reflux for 16 hours The mixture was cooled the supernatant liquid decanted from excess magnesium metal treated with sodium borohydride (3 g) and propan-2-ol (100 ml) The mixture was heated under reflux for 5 hours The reaction mixture was cooled added to water and excess concentrated hydrochloric acid was added The resulting solution was washed with toluene extracted with toluene The extracts were dried evaporated to give a residue which was distilled in a Buchi Kugelrohr apparatus (140°/0.4 mm)

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

实验步骤: 21.4 g Di-sodium tetra-iodoterephthalate, 0.5 g sodium iodide, and 10 g 2-chloropropanol were heated with stirring in 150 ml dimethylformamide at 100° C for 10 hours. The solvent was distilled off, and the residue was suspended in water and purified as described in Example 1. 14.15 g Bis-1-hydroxy-2-propyl ester of tetra-iodoterephthalic acid (60% yield) was recovered. It melted and decomposed at about 225° C. The solvent was distilled off purified