methylaminomethanetriol

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

实验步骤: Tri-hydroxymethylaminomethane (121.4 mg) and 412.5 mg of (E)-4-[[3-[2-(4-cyclobutyl-2-thiazolyl)-ethenyl]phenyl]amino]-2,2-diethyl-4-oxobutanoic acid were dissolved in 10 ml of ethanol. This solution was then condensed by rotary evaporation to yield (E)-4-[[3-[2-(4-cyclobutyl-2-thiazolyl)ethenyl]phenyl]amino]-2,2-diethyl-4-oxobutanoic acid tri-hydroxymethylaminomethane salt as a free flowing solid after trituration with cold acetonitrile, m.p. 80°-87° C. condensed by rotary evaporation

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

实验步骤: To a solution of 5 gm. of di(tris-hydroxymethyl) methylammonium 10-chloro-1,4,6,9-tetrahydro-4,6-dioxopyrido[4,3-g]quinoline-2,8-dicarboxylate in 100 ml. of water is added 2.0 g. of 5% palladium-on-charcoal catalyst and 5.0 g. of magnesium oxide. The resulting mixture is hydrogenated at an initial pressure of 3 atmospheres of hydrogen until 1 mole of hydrogen has been absorbed. The mixture is filtered and the filtrate acidified by the addition of dilute hydrochloric acid. The resulting precipitate is removed by filtration. The 1,4,6,9-tetrahydro-4,6-dioxopyrido[3,2-g]quinoline-2,8-dicarboxylic acid obtained is converted to di(tris-hydroxymethyl)methylammonium 1,4,6,9-tetrahydro-4,6-dioxopyrido[3,2-g]quinoline-2,8-dicarboxylate by adding two equivalents of (tris-hydroxymethyl)methylamine in aqueous solution. The crystalline product is recovered after addition of methanol. The crystalline product is recovered after addition of methanol

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

实验步骤: To a solution of 5 gm. of di(tris-hydroxymethyl) methylammonium 10-chloro-1,4,6,9-tetrahydro-4,6-dioxopyrido[4,3-g]quinoline-2,8-dicarboxylate in 100 ml. of water is added 2.0 g. of 5% palladium-on-charcoal catalyst and 5.0 g. of magnesium oxide. The resulting mixture is hydrogenated at an initial pressure of 3 atmospheres of hydrogen until 1 mole of hydrogen has been absorbed. The mixture is filtered and the filtrate acidified by the addition of dilute hydrochloric acid. The resulting precipitate is removed by filtration. The 1,4,6,9-tetrahydro-4,6-dioxopyrido[3,2-g]quinoline-2,8-dicarboxylic acid obtained is converted to di(tris-hydroxymethyl)methylammonium 1,4,6,9-tetrahydro-4,6-dioxopyrido[3,2-g]quinoline-2,8-dicarboxylate by adding two equivalents of (tris-hydroxymethyl)methylamine in aqueous solution. The crystalline product is recovered after addition of methanol. The crystalline product is recovered after addition of methanol

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

实验步骤: Tri-hydroxymethylaminomethane (121.4 mg) and 412.5 mg of (E)-4-[[3-[2-(4-cyclobutyl-2-thiazolyl)-ethenyl]phenyl]amino]-2,2-diethyl-4-oxobutanoic acid were dissolved in 10 ml of ethanol. This solution was then condensed by rotary evaporation to yield (E)-4-[[3-[2-(4-cyclobutyl-2-thiazolyl)ethenyl]phenyl]amino]-2,2-diethyl-4-oxobutanoic acid tri-hydroxymethylaminomethane salt as a free flowing solid after trituration with cold acetonitrile, m.p. 80°-87° C. condensed by rotary evaporation

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

实验步骤: Tri-hydroxymethylaminomethane (121.4 mg) and 412.5 mg of (E)-4-[[3-[2-(4-cyclobutyl-2-thiazolyl)-ethenyl]phenyl]amino]-2,2-diethyl-4-oxobutanoic acid were dissolved in 10 ml of ethanol. This solution was then condensed by rotary evaporation to yield (E)-4-[[3-[2-(4-cyclobutyl-2-thiazolyl)ethenyl]phenyl]amino]-2,2-diethyl-4-oxobutanoic acid tri-hydroxymethylaminomethane salt as a free flowing solid after trituration with cold acetonitrile, m.p. 80°-87° C. condensed by rotary evaporation

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

实验步骤: To a solution of 5 gm. of di(tris-hydroxymethyl) methylammonium 10-chloro-1,4,6,9-tetrahydro-4,6-dioxopyrido[4,3-g]quinoline-2,8-dicarboxylate in 100 ml. of water is added 2.0 g. of 5% palladium-on-charcoal catalyst and 5.0 g. of magnesium oxide. The resulting mixture is hydrogenated at an initial pressure of 3 atmospheres of hydrogen until 1 mole of hydrogen has been absorbed. The mixture is filtered and the filtrate acidified by the addition of dilute hydrochloric acid. The resulting precipitate is removed by filtration. The 1,4,6,9-tetrahydro-4,6-dioxopyrido[3,2-g]quinoline-2,8-dicarboxylic acid obtained is converted to di(tris-hydroxymethyl)methylammonium 1,4,6,9-tetrahydro-4,6-dioxopyrido[3,2-g]quinoline-2,8-dicarboxylate by adding two equivalents of (tris-hydroxymethyl)methylamine in aqueous solution. The crystalline product is recovered after addition of methanol. The crystalline product is recovered after addition of methanol

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

实验步骤: Tri-hydroxymethylaminomethane (121.4 mg) and 412.5 mg of (E)-4-[[3-[2-(4-cyclobutyl-2-thiazolyl)-ethenyl]phenyl]amino]-2,2-diethyl-4-oxobutanoic acid were dissolved in 10 ml of ethanol. This solution was then condensed by rotary evaporation to yield (E)-4-[[3-[2-(4-cyclobutyl-2-thiazolyl)ethenyl]phenyl]amino]-2,2-diethyl-4-oxobutanoic acid tri-hydroxymethylaminomethane salt as a free flowing solid after trituration with cold acetonitrile, m.p. 80°-87° C. condensed by rotary evaporation