2,2,3,3,4,4,4-heptafluorobutanal

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 3-necked round bottom flask fitted with dropping funnel, dry-ice condenser, and gas inlet was charged with 10% Pd/C(0.35 g) and cooled to 0° C. Triisopropylsilane (7.29 g, 46 mmol) was added, and CF3CF2CF2C(O)Cl (9.30 g, 40 mmol) was added dropwise over a 10 min period. The reactor was connected to a cold trap (-78° C.) while the mixture was stirred for 18 hr. Transfer from the trap and reaction vessel gave a total of 5.1 g (62%) of colorless liquid. 1H NMR (CD2Cl2): 9.62 (m). 19F NMR: -81.24 (t, J=8.3 Hz), -126.4 (quartet of doublets, Jq =8.3, Jd =3.2), -127.9 (s). A 3-necked round bottom flask fitted The reactor was connected to a cold trap Transfer from the trap and reaction vessel

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 3-necked round bottom flask fitted with dropping funnel, dry-ice condenser, and gas inlet was charged with 10% Pd/C(0.35 g) and cooled to 0° C. Triisopropylsilane (7.29 g, 46 mmol) was added, and CF3CF2CF2C(O)Cl (9.30 g, 40 mmol) was added dropwise over a 10 min period. The reactor was connected to a cold trap (-78° C.) while the mixture was stirred for 18 hr. Transfer from the trap and reaction vessel gave a total of 5.1 g (62%) of colorless liquid. 1H NMR (CD2Cl2): 9.62 (m). 19F NMR: -81.24 (t, J=8.3 Hz), -126.4 (quartet of doublets, Jq =8.3, Jd =3.2), -127.9 (s). A 3-necked round bottom flask fitted The reactor was connected to a cold trap Transfer from the trap and reaction vessel

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 3-necked round bottom flask fitted with dropping funnel, dry-ice condenser, and gas inlet was charged with 10% Pd/C(0.35 g) and cooled to 0° C. Triisopropylsilane (7.29 g, 46 mmol) was added, and CF3CF2CF2C(O)Cl (9.30 g, 40 mmol) was added dropwise over a 10 min period. The reactor was connected to a cold trap (-78° C.) while the mixture was stirred for 18 hr. Transfer from the trap and reaction vessel gave a total of 5.1 g (62%) of colorless liquid. 1H NMR (CD2Cl2): 9.62 (m). 19F NMR: -81.24 (t, J=8.3 Hz), -126.4 (quartet of doublets, Jq =8.3, Jd =3.2), -127.9 (s). A 3-necked round bottom flask fitted The reactor was connected to a cold trap Transfer from the trap and reaction vessel

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

実験手順: Pyrrole (2; 50 mmol) and heptafluorobutyraldehyde (7; R=CF3CF2, as the hydrate, 25 mmol) were condensed in tetrahydrofuran in the presence of acid catalyst as described above to give bis-(pyrrol-2-yl) heptafluoroprop-1-ylmethane (8; R=CF3CF2) in >50% isolated yield. GCMS m/z; 314 (M+, 22%), 145 (100%); 1H NMR (δ, CDCl3 at 7.24); 4.92 (t, 1H), 6.22 (d, 4H), 6.75 (s, 2H), 8.07 (bs, 2H).

反応条件: temp:0.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: A 3-necked round bottom flask fitted with with dropping funnel, dry-ice condenser, and gas inlet was charged with 10% Pd/C (0.35 g) and cooled to 0° C. Triisopropylsilane (7.29 g, 46 mmol) was added, and CF3CF2CF2C(O)Cl (9.30 g, 40 mmol) was added dropwise over a 10 min period. The reactor was connected to a cold trap (-78° C.) while the mixture was stirred for 18 hr. Transfer from the trap and reaction vessel gave a total of 5.1 g (62%) of colorless liquid. 1H NMR (CD2Cl2): 9.62 (m). 19F NMR: -81.24 (t, J=8.3 Hz), -126.4 (quartet of doublets, Jq =8.3, Jd =3.2), -127.9 (s). A 3-necked round bottom flask fitted with The reactor was connected to a cold trap Transfer from the trap and reaction vessel

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

実験手順: Pyrrole (2; 50 mmol) and heptafluorobutyraldehyde (7; R=CF3CF2, as the hydrate, 25 mmol ) were condensed in tetrahydrofuran in the presence of acid catalyst as described above to give bis-(pyrrol-2-yl) hepta-fluoroprop-1-ylmethane (8; R=CF3CF2) in >50% isolated yield. GCMS m/z; 314 (M+, 22%), 145 (100%); 1H NMR (δ, CDCl3 at 7.24); 4.92 (t, 1H), 6.22 (d, 4H), 6.75 (s, 2H), 8.07 (bs, 2H).

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

実験手順: Pyrrole (2; 50mmol) and heptafluorobutyraldehyde (7; R=CF3CF2, as the hydrate, 25 mmol) were condensed in tetrahydrofuran in the presence of acid catalyst as described above to give bis-(pyrrol-2-yl) heptafluoroprop-1-ylmethane (8; R=CF3CF2) in >50% isolated yield. GCMS m/z; 314 (M+, 22%), 145 (100%); 1H NMR (δ, CDCl3 at 7.24); 4.92 (t, 1H), 6.22 (d, 4H), 6.75 (s, 2H), 8.07 (bs, 2H).