[二]乙酸亞甲酯

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 1-liter, magnetically stirred autoclave was charged with 0.001 mol of Rh(CO)2Cl, sealed and flushed with nitrogen followed by carbon monoxide. The autoclave was then charged with 1 mol of methyl acetate, 1 mol of trioxane, 0.5 mol of acetic acid and 0.056 mol of hydrogen iodide. The autoclave was sealed, pressured to 1000 psig with carbon monoxide, and rapidly heated to 200° C. After 16 hours at 200° C., the reaction was terminated, the autoclave was opened and the reaction mixture analyzed by nuclear magnetic resonance spectroscopy, infrared spectroscopy and gas-liquid chromatography. The conversion of methyl acetate was 49% and the yield of methylene bis-acetate, ##STR9## based on converted methyl acetate, was 28%. sealed flushed with nitrogen The autoclave was sealed the reaction was terminated

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 1-liter, magnetically stirred autoclave was charged with 0.001 mol of Rh(CO)2Cl, sealed and flushed with nitrogen followed by carbon monoxide. The autoclave was then charged with 1 mol of methyl acetate, 1 mol of trioxane, 0.5 mol of acetic acid and 0.056 mol of hydrogen iodide. The autoclave was sealed, pressured to 1000 psig with carbon monoxide, and rapidly heated to 200° C. After 16 hours at 200° C., the reaction was terminated, the autoclave was opened and the reaction mixture analyzed by nuclear magnetic resonance spectroscopy, infrared spectroscopy and gas-liquid chromatography. The conversion of methyl acetate was 49% and the yield of methylene bis-acetate, ##STR9## based on converted methyl acetate, was 28%. sealed flushed with nitrogen The autoclave was sealed the reaction was terminated

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 1-liter, magnetically stirred autoclave was charged with 0.001 mol of Rh(CO)2Cl, sealed and flushed with nitrogen followed by carbon monoxide. The autoclave was then charged with 1 mol of methyl acetate, 1 mol of trioxane, 0.5 mol of acetic acid and 0.056 mol of hydrogen iodide. The autoclave was sealed, pressured to 1000 psig with carbon monoxide, and rapidly heated to 200° C. After 16 hours at 200° C., the reaction was terminated, the autoclave was opened and the reaction mixture analyzed by nuclear magnetic resonance spectroscopy, infrared spectroscopy and gas-liquid chromatography. The conversion of methyl acetate was 49% and the yield of methylene bis-acetate, ##STR9## based on converted methyl acetate, was 28%. sealed flushed with nitrogen The autoclave was sealed the reaction was terminated

反应条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 5 g of concentrated sulphuric acid are added dropwise to a suspension of 300 g of paraformaldehyde in 1,020 g of acetic anhydride in the course of 5 minutes, during which the temperature rises from room temperature to about 100° C. When the addition had ended, the mixture is heated to 150° C. and is stirred at this temperature for 3 hours. It is then cooled to room temperature, 25 g of sodium acetate are added and the volatile constituents are distilled off in vacuo. About 1,300 g of distillate are thereby obtained, and are then fractionated, with addition of 10 g of sodium acetate, over a 50 cm packed column. 1,150 g (87.1% of theory) of methylene diacetate of boiling point 96° to 99° C. under 90 mbar are thereby obtained. rises from room temperature to about 100° C When the addition It is then cooled to room temperature the volatile constituents are distilled off in vacuo About 1,300 g of distillate are thereby obtained

反应条件: temp:200.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A 1-liter, magnetically stirred autoclave was charged with 0.001 mol of Rh(CO)2Cl, sealed and flushed with nitrogen followed by carbon monoxide. The autoclave was then charged with 1 mol of methyl acetate, 1 mol of trioxane, 0.5 mol of acetic acid and 0.056 mol of hydrogen iodide. The autoclave was sealed, pressured to 1000 psig with carbon monoxide, and rapidly heated to 200° C. After 16 hours at 200° C., the reaction was terminated, the autoclave was opened and the reaction mixture analyzed by nuclear magnetic resonance spectroscopy, infrared spectroscopy and gas-liquid chromatography. The conversion of methyl acetate was 49% and the yield of methylene bis-acetate, ##STR9## based on converted methyl acetate, was 28%. sealed flushed with nitrogen The autoclave was sealed the reaction was terminated