2-乙基-2-甲基-1,3-丙二醇

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

实验步骤: A mixture of 590 g (5 moles) of 2-ethyl-2-methyl1,3-propanediol, 479 g (5.5 moles) of 85% strength methoxyacetaldehyde and 500 ml of chloroform was heated with 10 g of pyridinium p-toluenesulfonate under a water separator until water no longer separated off. The remaining solution was deionized using a mixed-bed ion exchanger, the solvent was removed under reduced pressure and the residue was distilled. 774 g (89% yield) of 2-methoxymethyl-5-ethyl-5-methyl-1,3-dioxane of boiling point 58° C./1 mbar were obtained. no longer separated off the solvent was removed under reduced pressure the residue was distilled

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

实验步骤: With 4-nitrobenzylphosphonic acid and 2-ethyl-2-methyl-1,3-propanediol, the same procedure as in Reference Example 11 was followed, to yield 5-ethyl-5-methyl-2-(4-nitrobenzyl)-1,3,2-dioxaphosphorinane-2-oxide, which was then recrystallized from ethanol-hexane to yield colorless prisms having a melting point of 184° to 185° C.

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

实验步骤: With 4-nitrobenzylphosphonic acid and 2-ethyl-2-methyl-1,3-propanediol, the same procedure as in Reference Example 11 was followed, to yield 5-ethyl-5-methyl-2-(4-nitrobenzyl)-1,3,2-dioxaphosphorinane-2-oxide, which was then recrystallized from ethanol-hexane to yield colorless prisms having a melting point of 184° to 185° C.

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

实验步骤: Using the method described in Example 1(b), one part per hour of a 70 percent strength by weight aqueous solution of 2-methyl-2-ethyl-3-hydroxypropanal is hydrogenated, over the catalyst prepared as described in Example 1(a), at 130° C. and 30 bar, with a throughput of 0.35 part of 2-methyl-2-ethyl-3-hydroxypropanal per liter of catalyst per hour. The conversion is 99 percent. The hydrogenated material is fractionated through a packed column. After first runnings of water and small amounts of methanol, 2-methylbutanol and 2-methyl-2-ethyl-3-hydroxypropanal, 2-methyl-2-ethyl-propane-1,3-diol, of boiling point of 110°-112° C./12 mbar (melting point 44°-46° C.), is obtained in an amount corresponding to 0.6850 part per hour. This is equivalent to a yield of 96.2% of theory, based on starting material. prepared as described in Example 1(a), at 130° C.

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

实验步骤: Amorphous poly (2-methyl-2 -ethyl-1,3-propylene sebacate) was prepared by reacting sebacic acid and a 10 mole % excess of 2-methyl-2-ethyl-1,3-propylene glycol in the presence of 0.5 weight % p-toluenesulfonic acid in the same manner as in Example 1. On cooling to room temperature after the polymerization, the poly (MEPS) remained as a clear, tacky fluid. Analysis indicates it has an acid number of 2.40, an hydroxyl number of 19.4, an Mn of 5150 g/mole, an MWD of 1.87 by GPC in chloroform, and a glass transition temperature of about -61°C. after the polymerization

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

实验步骤: 4-Nitrobenzylphosphonic acid and 2-ethyl-2-methyl-1,3-propanediol were treated in the same manner as in Reference Example 20 to yield 5-ethyl-5-methyl-2-(4-nitrobenzyl)-1,3,2-dioxaphosphorinan-2-oxide, which was then recrystallized from ethanol-hexane to yield colorless prisms having a melting point of 184°-185° C.

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

实验步骤: 126 g of α-ethylacrolein, 300 g of a 30% strength aqueous solution of formaldehyde, 1 g of hydroquinone and 350 g of 1,4-dioxane were combined at 25° C to give a solution. After about 2 hours, 120 g of this solution, which had a pH value of 2-3, were hydrogenated as in Example 1. Analysis of the hydrogenated product gave 55.9% of 2-ethyl-2-methylpropane-1,3-diol and 34% of methylbutanol, relative to the α-ethylacrolein employed. were combined at 25° C to give a solution

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

实验步骤: A mixture of 590 g (5 moles) of 2-ethyl-2-methyl1,3-propanediol, 479 g (5.5 moles) of 85% strength methoxyacetaldehyde and 500 ml of chloroform was heated with 10 g of pyridinium p-toluenesulfonate under a water separator until water no longer separated off. The remaining solution was deionized using a mixed-bed ion exchanger, the solvent was removed under reduced pressure and the residue was distilled. 774 g (89% yield) of 2-methoxymethyl-5-ethyl-5-methyl-1,3-dioxane of boiling point 58° C./1 mbar were obtained. no longer separated off the solvent was removed under reduced pressure the residue was distilled

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

实验步骤: A mixture of 590 g (5 moles) of 2-ethyl-2-methyl1,3-propanediol, 479 g (5.5 moles) of 85% strength methoxyacetaldehyde and 500 ml of chloroform was heated with 10 g of pyridinium p-toluenesulfonate under a water separator until water no longer separated off. The remaining solution was deionized using a mixed-bed ion exchanger, the solvent was removed under reduced pressure and the residue was distilled. 774 g (89% yield) of 2-methoxymethyl-5-ethyl-5-methyl-1,3-dioxane of boiling point 58° C./1 mbar were obtained. no longer separated off the solvent was removed under reduced pressure the residue was distilled

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

实验步骤: With 4-nitrobenzylphosphonic acid and 2-ethyl-2-methyl-1,3-propanediol, the same procedure as in Reference Example 11 was followed, to yield 5-ethyl-5-methyl-2-(4-nitrobenzyl)-1,3,2-dioxaphosphorinane-2-oxide, which was then recrystallized from ethanol-hexane to yield colorless prisms having a melting point of 184° to 185° C.

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

实验步骤: With 4-nitrobenzylphosphonic acid and 2-ethyl-2-methyl-1,3-propanediol, the same procedure as in Reference Example 11 was followed, to yield 5-ethyl-5-methyl-2-(4-nitrobenzyl)-1,3,2-dioxaphosphorinane-2-oxide, which was then recrystallized from ethanol-hexane to yield colorless prisms having a melting point of 184° to 185° C.

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

实验步骤: Using the method described in Example 1(b), one part per hour of a 70 percent strength by weight aqueous solution of 2-methyl-2-ethyl-3-hydroxypropanal is hydrogenated, over the catalyst prepared as described in Example 1(a), at 130° C. and 30 bar, with a throughput of 0.35 part of 2-methyl-2-ethyl-3-hydroxypropanal per liter of catalyst per hour. The conversion is 99 percent. The hydrogenated material is fractionated through a packed column. After first runnings of water and small amounts of methanol, 2-methylbutanol and 2-methyl-2-ethyl-3-hydroxypropanal, 2-methyl-2-ethyl-propane-1,3-diol, of boiling point of 110°-112° C./12 mbar (melting point 44°-46° C.), is obtained in an amount corresponding to 0.6850 part per hour. This is equivalent to a yield of 96.2% of theory, based on starting material. prepared as described in Example 1(a), at 130° C.