1,3-diazinane-2,4-dione

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: substituting 1-chloro-3-{4-[4-fluoro-2-(2,2,2-trifluoroethoxy)phenyl]piperazin-1-yl}propane and 5,6-dihydro-2,4(1H,3H)-pyrimidinedione and recrystallizing from a solution of hydrochloric acid in alcohol gave 3-(3-{4-[4-fluoro-2-(2,2,2-trifluoroethoxy)phenyl]piperazin-1-yl}propyl)-5,6-dihydro-2,4(1H,3H)-pyrimidinedione hydrochloride, m.p. 186°-189° C.; Anal.: Calcd. for C19H24F4N5O3.(HCl)2 : C, 44.10; H, 5.06; N, 10.83%; Found: C, 43.99; H, 5.16; N, 10.78%; and recrystallizing from a solution of hydrochloric acid in alcohol

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: substituting 1-chloro-3-{4-[4-fluoro-2-(2,2,2-trifluoroethoxy)phenyl]piperazin-1-yl}propane and 5,6-dihydro-2,4(1H,3H)-pyrimidinedione and recrystallizing from a solution of hydrochloric acid in alcohol gave 3-(3-{4-[4-fluoro-2-(2,2,2-trifluoroethoxy)phenyl]piperazin-1-yl}propyl)-5,6-dihydro-2,4(1H,3H)-pyrimidinedione hydrochloride, m.p. 186°-189° C.; Anal.: Calcd. for C19H24F4N5O3.(HCl)2 : C, 44.10; H, 5.06; N, 10.83%; Found: C, 43.99; H, 5.16; N, 10.78%; and recrystallizing from a solution of hydrochloric acid in alcohol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: substituting 1-chloro-3-{4-[4-fluoro-2-(2,2,2-trifluoroethoxy)phenyl]piperazin-1-yl}propane and 5,6-dihydro-2,4(1H,3H)-pyrimidinedione and recrystallizing from a solution of hydrochloric acid in alcohol gave 3-(3-{4-[4-fluoro-2-(2,2,2-trifluoroethoxy)phenyl]piperazin-1-yl}propyl)-5,6-dihydro-2,4(1H,3H)-pyrimidinedione hydrochloride, m.p. 186°-189° C.; Anal.: Calcd. for C19H24F4N5O3.(HCl)2 : C, 44.10; H, 5.06; N, 10.83%; Found: C, 43.99; H, 5.16; N, 10.78%; and recrystallizing from a solution of hydrochloric acid in alcohol

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: After adding 1.5 gm of finely pulverized sodium acetate suspended in 1 liter of ethyl acetate, 15 gm (0.13 mol) of 5,6-dihydrouracil were reacted with ketene at boiling temperature (77° C). After the reaction had been completed, the catalyst was filtered off and the solvent was distilled off under reduced pressure. The residue was recrystallized from isopropanol. The melting point was 81.5° C to 83° C, and the elementary analysis resulted in the following values: the catalyst was filtered off the solvent was distilled off under reduced pressure The residue was recrystallized from isopropanol The melting point was 81.5° C to 83° C, and the elementary analysis resulted in the following values

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 57 gm (0.5 mol) of 5,6-dihydrouracil and 817 gm (8 mols) of acetic acid anhydride were heated to boiling for ten hours after adding 2 ml of concentrated sulfuric acid thereto. The acetic acid produced was continuously distilled off by means of a fractionating column. After the acylation reaction had been completed, the surplus acetic acid anhydride was distilled off in vacuo (15 Torr) and the residue was recrystallized from isopropanol. The product obtained had a melting point of 191° to 193° C, and the elementary analysis resulted in the following values: to boiling for ten hours was continuously distilled off by means of a fractionating column After the acylation reaction the surplus acetic acid anhydride was distilled off in vacuo (15 Torr) the residue was recrystallized from isopropanol The product obtained the elementary analysis resulted in the following values

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 57 gm (0.5 mol) of 5,6-dihydrouracil and 817 gm (8 mols) of acetic acid anhydride were heated to boiling for ten hours after adding 2 ml of concentrated sulfuric acid thereto. The acetic acid produced was continuously distilled off by means of a fractionating column. After the acylation reaction had been completed, the surplus acetic acid anhydride was distilled off in vacuo (15 Torr) and the residue was recrystallized from isopropanol. The product obtained had a melting point of 191° to 193° C, and the elementary analysis resulted in the following values: to boiling for ten hours was continuously distilled off by means of a fractionating column After the acylation reaction the surplus acetic acid anhydride was distilled off in vacuo (15 Torr) the residue was recrystallized from isopropanol The product obtained the elementary analysis resulted in the following values

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Adopting the procedure outlined for example 9 using 40.0 mg (0.12 mmol) of {4-[1-(3,5,5,8,8-Pentamethyl-5,6,7,8-tetrahydro-naphthalen-2-yl)-vinyl]-phenyl}-methanol, 0.05 mL of methanesulfonyl chloride, 0.10 mL of NEt3, 300 mg of dihydropyrimidine-2,4-dione, and 63 mg of NaH, 28.4 mg of the product was obtained.