-4-特丁基噁唑啉-2-酮

反应条件: temp:65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 73 g (containing 0.25 mole (R)-tert-leucinol) of the filtrate cited in example 6 was taken up with 27 ml water and 200 ml toluene. 25 ml (0.26 mole) chloroformic acid ethyl ester were then added dropwise at 20°-25° C., during which the pH was maintained at 7-8.5 by the addition of 10 M sodium hydroxide solution. The mixture was then heated to 60°-65° C. at pH 8.0 and the aqueous phase separated. The toluene phase was dehydrated on a water separator under a slight vacuum and slowly heated after the addition of 0.4 g finely granulated sodium hydroxide at 70° C. A total of 40 ml distillate which contained the ethanol produced during the reaction was separated from 70°-100° C . After cooling of the batch to 65° C. a solution of 0.6 ml glacial acetic acid in 10 ml water was added, the mixture briefly agitated, the aqueous phase separated and the toluene phase compounded again with 15 ml warm water which was separated again after a brief agitation at 65° C. After distilling the organic phase on a water separator the phase was concentrated to 120 ml, filtered hot and slowly cooled off under agitation, during which the product separated in colorless crystals. These crystals were filtered off after 30 min agitation at 5° C., washed with cold toluene and dried in a vacuum at 50° C. 28.6 g (R)-4-tert-butyl-2-oxazolidinone (80% yield) was obtained. A 1H-NMR spectrum corroborated the structure of the product. The mixture was then heated to 60°-65° C. at pH 8.0 the aqueous phase separated slowly heated after the addition of 0.4 g finely granulated sodium hydroxide at 70° C produced during the reaction was separated from 70°-100° C was added the aqueous phase separated warm water which was separated again after a brief agitation at 65° C After distilling the organic phase on a water separator the phase was concentrated to 120 ml filtered hot slowly cooled off under agitation, during which the product separated in colorless crystals These crystals were filtered off after 30 min agitation at 5° C. washed with cold toluene dried in a vacuum at 50° C

反应条件: temp:65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 73 g (containing 0.25 mole (R)-tert-leucinol) of the filtrate cited in example 6 was taken up with 27 ml water and 200 ml toluene. 25 ml (0.26 mole) chloroformic acid ethyl ester were then added dropwise at 20°-25° C., during which the pH was maintained at 7-8.5 by the addition of 10 M sodium hydroxide solution. The mixture was then heated to 60°-65° C. at pH 8.0 and the aqueous phase separated. The toluene phase was dehydrated on a water separator under a slight vacuum and slowly heated after the addition of 0.4 g finely granulated sodium hydroxide at 70° C. A total of 40 ml distillate which contained the ethanol produced during the reaction was separated from 70°-100° C . After cooling of the batch to 65° C. a solution of 0.6 ml glacial acetic acid in 10 ml water was added, the mixture briefly agitated, the aqueous phase separated and the toluene phase compounded again with 15 ml warm water which was separated again after a brief agitation at 65° C. After distilling the organic phase on a water separator the phase was concentrated to 120 ml, filtered hot and slowly cooled off under agitation, during which the product separated in colorless crystals. These crystals were filtered off after 30 min agitation at 5° C., washed with cold toluene and dried in a vacuum at 50° C. 28.6 g (R)-4-tert-butyl-2-oxazolidinone (80% yield) was obtained. A 1H-NMR spectrum corroborated the structure of the product. The mixture was then heated to 60°-65° C. at pH 8.0 the aqueous phase separated slowly heated after the addition of 0.4 g finely granulated sodium hydroxide at 70° C produced during the reaction was separated from 70°-100° C was added the aqueous phase separated warm water which was separated again after a brief agitation at 65° C After distilling the organic phase on a water separator the phase was concentrated to 120 ml filtered hot slowly cooled off under agitation, during which the product separated in colorless crystals These crystals were filtered off after 30 min agitation at 5° C. washed with cold toluene dried in a vacuum at 50° C

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

实验步骤: By reaction and treatment in the same manner as in Example 1 and using (4-bromo-2-methanesulfonylphenyl)[4-(2,4-dimethylphenyl)piperazin-1-yl]methanone (903 mg) described in Preparation Example 9 and (R)-4-tert-butyloxazolidin-2-one (286 mg), the title compound (9 mg) was obtained. By reaction and treatment in the same manner as in Example 1

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

实验步骤: To a mixture of [4-(2,4-dimethylphenyl)piperazin-1-yl](4-iodophenyl)methanone (841 mg) described in Preparation Example 8, (R)-(+)-4-tert-butyloxazolidin-2-one (214 mg), potassium carbonate (553 mg) and copper (I) iodide (76 mg) were added toluene (2 mL) and N,N′-dimethylethylenediamine (100 μL), and the mixture was refluxed for 8 hr. After cooling, water was added to the reaction mixture, and the mixture was extracted with chloroform. The organic layer was washed with saturated brine, and the solvent was evaporated. The residue was purified by column chromatography (chloroform:methanol) to give the title compound (7 mg). the mixture was refluxed for 8 hr After cooling the mixture was extracted with chloroform The organic layer was washed with saturated brine the solvent was evaporated The residue was purified by column chromatography (chloroform:methanol)

反应条件: temp:65.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 73 g (containing 0.25 mole (R)-tert-leucinol) of the filtrate cited in example 6 was taken up with 27 ml water and 200 ml toluene. 25 ml (0.26 mole) chloroformic acid ethyl ester were then added dropwise at 20°-25° C., during which the pH was maintained at 7-8.5 by the addition of 10 M sodium hydroxide solution. The mixture was then heated to 60°-65° C. at pH 8.0 and the aqueous phase separated. The toluene phase was dehydrated on a water separator under a slight vacuum and slowly heated after the addition of 0.4 g finely granulated sodium hydroxide at 70° C. A total of 40 ml distillate which contained the ethanol produced during the reaction was separated from 70°-100° C . After cooling of the batch to 65° C. a solution of 0.6 ml glacial acetic acid in 10 ml water was added, the mixture briefly agitated, the aqueous phase separated and the toluene phase compounded again with 15 ml warm water which was separated again after a brief agitation at 65° C. After distilling the organic phase on a water separator the phase was concentrated to 120 ml, filtered hot and slowly cooled off under agitation, during which the product separated in colorless crystals. These crystals were filtered off after 30 min agitation at 5° C., washed with cold toluene and dried in a vacuum at 50° C. 28.6 g (R)-4-tert-butyl-2-oxazolidinone (80% yield) was obtained. A 1H-NMR spectrum corroborated the structure of the product. The mixture was then heated to 60°-65° C. at pH 8.0 the aqueous phase separated slowly heated after the addition of 0.4 g finely granulated sodium hydroxide at 70° C produced during the reaction was separated from 70°-100° C was added the aqueous phase separated warm water which was separated again after a brief agitation at 65° C After distilling the organic phase on a water separator the phase was concentrated to 120 ml filtered hot slowly cooled off under agitation, during which the product separated in colorless crystals These crystals were filtered off after 30 min agitation at 5° C. washed with cold toluene dried in a vacuum at 50° C