4-methyl-1,3-dioxolan-2-one

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:

反応条件: temp:60.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: To a solution of diethylfluorene (22.2 g., 0.1 mol.) in propylene carbonate (100 ml), N-bromosuccinimide (17.8 g., 0.1 mol.) was added at 57° C. in portions and the mixture was stirred for 30 minutes at 60° C. The mixture was diluted with 1200 ml of water and extracted with 500 ml of toluene. The toluene extract was washed 3 times with 300 ml portions of water, dried and concentrated. The crude product from 3 batches of the same size totaled 117 g. of oil. This was distilled at 2 mm. The first fraction, b.p. 90-93° C., 22.33 g. was found to be propylene carbonate. The second fraction, b. p. 155-165° C., 81.0 g. (89.7% yield) was the desired product. Mass Spec: (m/z): 300, 302 (M+). extracted with 500 ml of toluene The toluene extract was washed 3 times with 300 ml portions of water dried concentrated This was distilled at 2 mm

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: 4-methyl-1,3-dioxolan-2-one and propylene oxide were reacted in a similar manner to the procedure of Example 2, whereby 2,7-dimethyl-1,4,6,9-tetraoxaspiro[4.4]nonane was obtained in yield of about 70%.

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

実験手順: The pre-polymer solution of Example 13 A was diluted to 7% by weight polymer with propylene carbonate. The pre-polymer solution was made 30 millimolar in Tinuvin p, 17 millimolar in 1,1′-d-(3-phenyl(n-propyl)-4,4′ bipyridinium and 14 millimolar in 5,10-dihydro-5,10-dimethlphenazine simply by dissolving appropriate amounts of these materials in the pre-polymer solution. This solution was degassed by vacuum and flushed with nitrogen. Sufficient tolylene 2,4-diisocyanate (available from Aldrich Chemical Company, Inc. Milwaukee, Wis.) crosslinker was added to crosslink approximately 50 percent of the theoretical hydroxyl position. This solution was thoroughly mixed to ensure that the crosslinker was evenly distributed throughout the fluid. This solution was degassed by vacuum flushed with nitrogen Sufficient tolylene 2,4-diisocyanate (available from Aldrich Chemical Company, Inc. Milwaukee, Wis.) crosslinker was added This solution was thoroughly mixed

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

実験手順: The pre-polymer solution of Example 13 A was diluted to 7% by weight polymer with propylene carbonate. The pre-polymer solution was made 30 millimolar in Tinuvin p, 17 millimolar in 1,1′-d-(3-phenyl(n-propyl)-4,4′ bipyridinium and 14 millimolar in 5,10-dihydro-5,10-dimethlphenazine simply by dissolving appropriate amounts of these materials in the pre-polymer solution. This solution was degassed by vacuum and flushed with nitrogen. Sufficient tolylene 2,4-diisocyanate (available from Aldrich Chemical Company, Inc. Milwaukee, Wis.) crosslinker was added to crosslink approximately 50 percent of the theoretical hydroxyl position. This solution was thoroughly mixed to ensure that the crosslinker was evenly distributed throughout the fluid. This solution was degassed by vacuum flushed with nitrogen Sufficient tolylene 2,4-diisocyanate (available from Aldrich Chemical Company, Inc. Milwaukee, Wis.) crosslinker was added This solution was thoroughly mixed

反応条件: temp:131.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A mixture of 861 parts of isophorone diisocyanate, 535.95 parts of propylene carbonate and 2.15 parts of Dabco TMR* is stirred and gradually heated. When the temperature reaches 55° C. heating is discontinued. The exothermic reaction raises the temperature to 131° C. in 15 minutes. After cooling to 89° C., 5.8 parts of a 10% solution of Dabco TMR* in propylene carbonate is added. The temperature rises to 90° C. in 8 minutes. After heating to 132° C. it is allowed to cool. 1397.1 parts of this product, the tri-isocyanato-isocyanurate formed from 3 moles of isophorone di-isocyanate as a 61.4% solids solution in propylene carbonate, having an NCO content of 10.94% is stirred while 366.8 parts of 3,5-dimethylpyrazole is added, cooling as required, to keep the temperature below 80° C. followed by 463.4 parts of the monomethyl ether of propylene glycol. The mixture is stirred at 50° C. and a clear solution formed which solution is then allowed to cool. The IR Spectrum shows NCO absent. gradually heated reaches 55° C. heating The exothermic reaction After cooling to 89° C. After heating to 132° C. it to cool

反応条件: temp:140.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N,N′-Diphenylurea (20.7 g, 98.0 mmol) was dissolved in dimethyl sulfoxide (40 mL), and thereto were added cesium fluoride (1.48 g, 9.80 mmol) and 4-methyl-1,3-dioxolan-2-one (10.0 g, 98.0 mmol), in order. The mixture was stirred for 30 hours at 140° C. under an atmosphere of argon. After filtering off the insoluble materials, the filtrate was condensed in vacuo, and the residue was recrystallized from ethanol to give the subject 3-phenyl-5-methyloxazolidin-2-one (12.9 g, yield 74.3%). After filtering off the insoluble materials condensed in vacuo the residue was recrystallized from ethanol