苯巴比妥杂质5

反应条件: temp:2.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of 5-benzylbarbituric Acid (1.7 g) in 15 ml of water, cooled to 0-5° C. 1 ml of 48% hydrobromic acid are added followed by the addition dropwise of 0.437 ml of bromine into the reaction mixture. After 1 hour under stirring at a temperature below 10° C. the solid which formed is separated by filtration and washed with water. 2.17 g of the product are obtained, m.p. 164-166° C. formed is separated by filtration washed with water

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

实验步骤: To a suspension of 5-benzylidenebarbituric Acid (4 g) in 200 ml of methanol are added portionwise 1.4 g of sodium borohydride. After 10 minutes from the end of the addition, 100 ml of water are added and the mixture is acidified with 1 N hydrochloric acid to pH=2. The solvent is evaporated off and the aqueous phase is extracted with ethyl acetate. The pooled extracts are dried over sodium sulfate and concentrated to dryness. 3.6 g of the product crystallize, m.p. 207-209° C. are added The solvent is evaporated off the aqueous phase is extracted with ethyl acetate The pooled extracts are dried over sodium sulfate concentrated to dryness 3.6 g of the product crystallize

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

实验步骤: A solution of methanesulfonyl chloride (1.4 ml) in DMF (20 ml) was dropped into a stirred suspension of the triethylammonium salt of 5-benzyl-2,4,6-(1H,3H)-pyrimidinetrione (g 5) in DMF (210 ml). After an hour most of the solvent was removed in vacuo. The residual suspension was then poured into a ice-water mixture, and the precipitated white solid was collected by filtration, to yield, after drying, the title product, (4 g, 36.2% yield). After an hour most of the solvent was removed in vacuo The residual suspension was then poured into a ice-water mixture the precipitated white solid was collected by filtration to yield after drying

反应条件: temp:2.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of 5-benzylbarbituric acid (1.7 g) in 15 ml of water, cooled to 0-5° C., 1 ml of 48% hydrobromic acid are added followed by the addition dropwise of 0.437 ml of bromine into the reaction mixture. After 1 hour under stirring at a temperature below 10° C. the solid which formed is separated by filtration and washed with water. 2.17 g of the product are obtained. m.p. 164-166° C. formed is separated by filtration washed with water

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

实验步骤: To a suspension of 5-benzylidenebarbituric acid (4 g) in 200 ml of methanol are added portionwise 1.4 g of sodium borohydride. After 10 minutes from the end of the addition, 100 ml of water are added and the mixture is acidified with 1 N hydrochloric acid to pH=2. The solvent is evaporated off and the aqueous phase is extracted with ethyl acetate. The pooled extracts are dried over sodium sulfate and concentrated to dryness. 3.6 g of the product crystallize, m.p. 207-209° C. are added The solvent is evaporated off the aqueous phase is extracted with ethyl acetate The pooled extracts are dried over sodium sulfate concentrated to dryness 3.6 g of the product crystallize

反应条件: temp:2.51; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a suspension of 5-benzylbarbituric Acid (1.7 g) in 15 ml of water, cooled to 0-5° C. 1 ml of 48% hydrobromic acid are added followed by the addition dropwise of 0.437 ml of bromine into the reaction mixture. After 1 hour under stirring at a temperature below 10° C. the solid which formed is separated by filtration and washed with water. 2.17 g of the product are obtained, m.p. 164-166° C. formed is separated by filtration washed with water

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

实验步骤: To a suspension of 5-benzylidenebarbituric Acid (4 g) in 200 ml of methanol are added portionwise 1.4 g of sodium borohydride. After 10 minutes from the end of the addition, 100 ml of water are added and the mixture is acidified with 1 N hydrochloric acid to pH=2. The solvent is evaporated off and the aqueous phase is extracted with ethyl acetate. The pooled extracts are dried over sodium sulfate and concentrated to dryness. 3.6 g of the product crystallize, m.p. 207-209° C. are added The solvent is evaporated off the aqueous phase is extracted with ethyl acetate The pooled extracts are dried over sodium sulfate concentrated to dryness 3.6 g of the product crystallize