二乙氧基甲烷

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

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

实验步骤: 13.4 g of commercial 1,2,6-hexanetriol are added to 12.4 ml of diethoxymethane and the mixture is refluxed in the presence of 500 mg of toluenesulfonic acid acting as a transacetalisation catalyst. The ethanol is evaporated at 80° C. and the 4-(4-hydroxybutyl)-1,2-dioxolane obtained is purified by distillation. 7.3 g of this product and 4.6 g of epichlorhydrine are reacted in the presence of 2.8 g of potassium hydroxide (powder) and tetrabutylammonium chloride, to form the monomer 4-[(4-glycidyloxy)-butyl]-1,3-dioxolane The ethanol is evaporated at 80° C.

反应条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Preferred solvents include ethereals such as THF, diethoxymethane and t-butylmethyl ether. At about 0° C., a strong base is added dropwise over a period of about 15 minutes. Examples of strong bases are n-butyl lithium and lithium diisopropyl amide. While still maintaining the temperature near 0° C., a solution of allyl isocyanate in solvent is added dropwise over about 15 minutes. This is followed by the dropwise addition of trimethylsilyl chloride. After holding the reaction mixture at about 0 to about 10° C. for about 3 hours, the reaction is quenched with aqueous ammonium chloride and extracted with dichloromethane. The solvent is evaporated to yield the product, N-allyl-3-trimethylsilylpropiolic amide. ##STR8## wherein TMS is trimethylsilyl, the solvents are methylene chloride or DCE (1,2-dichloroethane), and the acid catalysts are aluminum chloride (AlCl3), ferric chloride (FeCl3) or methanesulfonic acid (MeSO3). At about 0° C., a strong base is added dropwise over a period of about 15 minutes at about 0 to about 10° C. for about 3 hours the reaction is quenched with aqueous ammonium chloride extracted with dichloromethane The solvent is evaporated

反应条件: temp:100.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A reaction flask was charged with 300 g (1.4 mole) 1,1,2,3,3-pentamethyl-hexahydro-4-indanol, 258 g (2.5 mole) diethoxymethane, 0.25 liter toluene, and 5 g boron trifluoride etherate complex. The reaction mass was heated to 100° C. and methanol and lite organics were collected in a Dean Stark trap (190 g recovered). After aging the reaction for 2 hrs the reaction was cooled to 25° C. and acid catalyst was quenched with 100 g of 10% aqueous sodium carbonate. The mass was transferred to a separatory funnel and water washed. The organic layer was separated and purified by fractional distillation. The procedure afforded a 68% yield (256 g) of 1,1,2,3,3-pentamethyl-octahydro-4-(ethoxymethoxy)-1H-indene. methanol and lite organics were collected in a Dean Stark trap (190 g recovered) the reaction for 2 hrs the reaction was cooled to 25° C. acid catalyst was quenched with 100 g of 10% aqueous sodium carbonate The mass was transferred to a separatory funnel water washed The organic layer was separated purified by fractional distillation

反应条件: temp:95.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: With stirring and under a nitrogen atmosphere 4-chloro-2-nitroaniline (5 g, 28.9 mmole) was dissolved in diethylphosphite (21.44 g, 155 mmole), followed by the addition of a solution of sulfuric acid (0.1 mL) and water (0.1 mL). Under a continuous flow of nitrogen the solution was heated to 95° C., after which diethoxymethane (9.05 g, 86.8 mmole) was added in a dropwise manner over a period of 1.5 hours while maintaining the temperature between 93°-97° C. Once all the diethoxymethane was added, the reaction was kept at 95°-105° C. for another hour after which the mixture was cooled to 45°-50° C. and cold water (70 mL) was added over 20 minutes. The resulting suspension was filtered, washed first with water (10 mL), then with heptane (10 mL). The obtained orange solid was dried at 30°-40° C. for 16 hours to yield 8.85 g (95%) of the title compound, mp 94°-5° C. while maintaining the temperature between 93°-97° C the reaction was kept at 95°-105° C. for another hour after which the mixture was cooled to 45°-50° C. The resulting suspension was filtered washed first with water (10 mL) The obtained orange solid was dried at 30°-40° C. for 16 hours

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir: