2-(trifluoromethyl)-1,3-dioxolane

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: This example illustrates a process of the invention only. A suspension of 9.6 g (0.20 mol) of 50% NaH in mineral oil in 150 mL of DM$0 was stirred at 15°-20° while 35.4 g (0.20 mol) of 2-chloroethyl trifluoroacetate were added dropwise. The resulting mixture was stirred overnight while the reaction temperature was maintained below 30° . The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) to drive off volatile products which were recovered. Fractionation of the volatiles gave 8.5 g (30% yield) of 2-trifluoromethyl-1,3-dioxolane, b.p. 87°-93° . IR (CCl4): 3000 and 2910 (sat'd CH), 1200-1100 cm-1 (CF,C--O). NMR (CCl4): 1H 5.13 (q, JHF 4Hz, IH, CH) and 4.07 ppm (s, 4H, ring OCH2). Anal.: Calcd. for C4H5F3O2 : C, 33.81; H, 3.55. Found: C, 33.68; H, 3.39 were added dropwise was maintained below 30° The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) were recovered

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

実験手順: This example illustrates a process of the invention only. A suspension of 9.6 g (0.20 mol) of 50% NaH in mineral oil in 150 mL of DMSO was stirred at 15°-20° while 35.4 g (0.20 mol) of 2-chloroethyl trifluoroacetate were added dropwise. The resulting mixture was stirred overnight while the reaction temperature was maintained below 30°. The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) to drive off volatile products which were recovered. Fractionation of the volatiles gave 8.5 g (30% yield) of 2-trifluoromethyl-1,3-dioxolane, b.p. 87°-93°. IR (CCl4): 3000 and 2910 (sat'd CH), 1200-1100 cm-1 (CF, C--O). NMR (CCl4): 1H 5.13 (q, JHF 4Hz, 1H, CH) and 4.07 ppm (s, 4H, ring OCH2). Anal.: Calcd. for C4H5F3O2 : C, 33.81; H, 3.55. Found: C, 33.68; H, 3.39 were added dropwise was maintained below 30° The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) were recovered

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

実験手順: This example illustrates a process of the invention only. A suspension of 9.6 g (0.20 mol) of 50% NaH in mineral oil in 150 mL of DMSO was stirred at 15°-20° while 35.4 g (0.20 mol) of 2-chloroethyl trifluoroacetate were added dropwise. The resulting mixture was stirred overnight while the reaction temperature was maintained below 30°. The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) to drive off volatile products which were recovered. Fractionation of the volatiles gave 8.5 g (30% yield) of 2-trifluoromethyl-1,3-dioxolane, b.p. 87°-93°. IR (CCl4): 3000 and 2910 (sat'd CH), 1200-1100 cm-1 (CF, C--O). NMR (CCl4): 1H 5.13 (q, JHF 4Hz, 1H, CH) and 4.07 ppm (s, 4H, ring OCH2). Anal.: Calcd. for C4H5F3O2 : C, 33.81; H, 3.55. Found: C, 33.68; H, 3.39 were added dropwise was maintained below 30° The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) were recovered

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

実験手順: This example illustrates a process of the invention only. A suspension of 9.6 g (0.20 mol) of 50% NaH in mineral oil in 150 mL of DMSO was stirred at 15°-20° while 35.4 g (0.20 mol) of 2-chloroethyl trifluoroacetate were added dropwise. The resulting mixture was stirred overnight while the reaction temperature was maintained below 30°. The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) to drive off volatile products which were recovered. Fractionation of the volatiles gave 8.5 g (30% yield) of 2-trifluoromethyl-1,3-dioxolane, b.p. 87°-93°. IR (CCl4): 3000 and 2910 (sat'd CH), 1200-1100 cm-1 (CF, C--O). NMR (CCl4): 1H 5.13 (q, JHF 4Hz, 1H, CH) and 4.07 ppm (s, 4H, ring OCH2). Anal.: Calcd. for C4H5F3O2 : C, 33.81; H, 3.55. Found: C, 33.68; H, 3.39 were added dropwise was maintained below 30° The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) were recovered

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

実験手順: This example illustrates a process of the invention only. A suspension of 9.6 g (0.20 mol) of 50% NaH in mineral oil in 150 mL of DMSO was stirred at 15°-20° while 35.4 g (0.20 mol) of 2-chloroethyl trifluoroacetate were added dropwise. The resulting mixture was stirred overnight while the reaction temperature was maintained below 30°. The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) to drive off volatile products which were recovered. Fractionation of the volatiles gave 8.5 g (30% yield) of 2-trifluoromethyl-1,3-dioxolane, b.p. 87°-93°. IR (CCl4): 3000 and 2910 (sat'd CH), 1200-1100 cm-1 (CF, C--O). NMR (CCl4): 1H 5.13 (q, JHF 4Hz, 1H, CH) and 4.07 ppm (s, 4H, ring OCH2). Anal.: Calcd. for C4H5F3O2 : C, 33.81; H, 3.55. Found: C, 33.68; H, 3.39 were added dropwise was maintained below 30° The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) were recovered

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

実験手順: This example illustrates a process of the invention only. A suspension of 9.6 g (0.20 mol) of 50% NaH in mineral oil in 150 mL of DM$0 was stirred at 15°-20° while 35.4 g (0.20 mol) of 2-chloroethyl trifluoroacetate were added dropwise. The resulting mixture was stirred overnight while the reaction temperature was maintained below 30° . The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) to drive off volatile products which were recovered. Fractionation of the volatiles gave 8.5 g (30% yield) of 2-trifluoromethyl-1,3-dioxolane, b.p. 87°-93° . IR (CCl4): 3000 and 2910 (sat'd CH), 1200-1100 cm-1 (CF,C--O). NMR (CCl4): 1H 5.13 (q, JHF 4Hz, IH, CH) and 4.07 ppm (s, 4H, ring OCH2). Anal.: Calcd. for C4H5F3O2 : C, 33.81; H, 3.55. Found: C, 33.68; H, 3.39 were added dropwise was maintained below 30° The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) were recovered

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

実験手順: This example illustrates a process of the invention only. A suspension of 9.6 g (0.20 mol) of 50% NaH in mineral oil in 150 mL of DM$0 was stirred at 15°-20° while 35.4 g (0.20 mol) of 2-chloroethyl trifluoroacetate were added dropwise. The resulting mixture was stirred overnight while the reaction temperature was maintained below 30° . The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) to drive off volatile products which were recovered. Fractionation of the volatiles gave 8.5 g (30% yield) of 2-trifluoromethyl-1,3-dioxolane, b.p. 87°-93° . IR (CCl4): 3000 and 2910 (sat'd CH), 1200-1100 cm-1 (CF,C--O). NMR (CCl4): 1H 5.13 (q, JHF 4Hz, IH, CH) and 4.07 ppm (s, 4H, ring OCH2). Anal.: Calcd. for C4H5F3O2 : C, 33.81; H, 3.55. Found: C, 33.68; H, 3.39 were added dropwise was maintained below 30° The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) were recovered

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: This example illustrates a process of the invention only. A suspension of 9.6 g (0.20 mol) of 50% NaH in mineral oil in 150 mL of DMSO was stirred at 15°-20° while 35.4 g (0.20 mol) of 2-chloroethyl trifluoroacetate were added dropwise. The resulting mixture was stirred overnight while the reaction temperature was maintained below 30°. The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) to drive off volatile products which were recovered. Fractionation of the volatiles gave 8.5 g (30% yield) of 2-trifluoromethyl-1,3-dioxolane, b.p. 87°-93°. IR (CCl4): 3300 and 2910 (sat'd CH), 1200-1100 cm-1 (CF, C--O). NMR (CCl4): 1H 5.13 (q, JHF 4 Hz, 1H, CH) and 4.07 ppm (s, 4H, ring OCH2). were added dropwise was maintained below 30° The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) were recovered

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

実験手順: This example illustrates a process of the invention only. A suspension of 9.6 g (0.20 mol) of 50% NaH in mineral oil in 150 mL of DMSO was stirred at 15°-20° while 35.4 g (0.20 mol) of 2-chloroethyl trifluoroacetate were added dropwise. The resulting mixture was stirred overnight while the reaction temperature was maintained below 30°. The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) to drive off volatile products which were recovered. Fractionation of the volatiles gave 8.5 g (30% yield) of 2-trifluoromethyl-1,3-dioxolane, b.p. 87°-93°. IR (CCl4): 3000 and 2910 (sat'd CH), 1200-1100 cm-1 (CF, C--O). NMR (CCl4): 1H 5.13 (q, JHF 4Hz, 1H, CH) and 4.07 ppm (s, 4H, ring OCH2). Anal.: Calcd. for C4H5F3O2 : C, 33.81; H, 3.55. Found: C, 33.68; H, 3.39 were added dropwise was maintained below 30° The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) were recovered

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

実験手順: This example illustrates a process of the invention only. A suspension of 9.6 g (0.20 mol) of 50% NaH in mineral oil in 150 mL of DMSO was stirred at 15°-20° while 35.4 g (0.20 mol) of 2-chloroethyl trifluoroacetate were added dropwise. The resulting mixture was stirred overnight while the reaction temperature was maintained below 30°. The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) to drive off volatile products which were recovered. Fractionation of the volatiles gave 8.5 g (30% yield) of 2-trifluoromethyl-1,3-dioxolane, b.p. 87°-93°. IR (CCl4): 3000 and 2910 (sat'd CH), 1200-1100 cm-1 (CF, C--O). NMR (CCl4): 1H 5.13 (q, JHF 4Hz, 1H, CH) and 4.07 ppm (s, 4H, ring OCH2). Anal.: Calcd. for C4H5F3O2 : C, 33.81; H, 3.55. Found: C, 33.68; H, 3.39 were added dropwise was maintained below 30° The reaction mixture was then heated to 50° at 0.33 kPa (2.5 mm) were recovered