Carbon–Carbon Bond Formation by Radical Cyclization
Data
1885
Compound 5a. Yield: 95%; white solid; mp 85–878C; IR (KBr): 2923,
1676, 1488, 754 cm21
;
1H NMR (CDCl3, 500 MHz): dH ¼ 2.89 (d, 1H,
J ¼ 16 Hz, –COCH), 2.95 (d, 1H, J ¼ 16 Hz, –COCH), 3.42 (s, 3H,
–NCH3), 3.75 (s, 3H, –OCH3), 4.30 (d, 1H, J ¼ 9 Hz, –OCH), 4.53
(d, 1H, J ¼ 9 Hz, –OCH), 6.66-7.33 (m, 7H, ArH); 13C NMR (CDCl3,
125 MHz): dC ¼ 28.97 (NCH3), 41.78 (CH2CO), 48.27 (CH2C), 55.44
(OCH3), 81.59 (OCH2), 109.31 (ArCH), 109.90 (ArCH), 114.06 (ArCH),
114.62 (ArCH), 122.97 (ArCH), 125.99 (ArCH), 127.98 (ArCH), 129.61
(ArC), 130.74 (ArC), 139.18 (ArC), 153.71 (ArC), 154.22 (ArC), 167.18
(CO); MS: m/z ¼ 295 (Mþ); UV (EtOH): lmax ¼ 302, 253, 210 nm. Anal.
calcd. for C18H17NO3: C, 73.20; H, 5.80; N, 4.74. Found: C, 73.49; H,
6.02; N, 4.53.
Compound 5b. Yield: 95%; white solid; mp 170–1728C; IR (KBr): 2922,
1678, 1451, 766 cm21
;
1H NMR (CDCl3, 400 MHz): dH ¼ 2.94 (d, 1H,
J ¼ 16 Hz, –COCH), 3.05 (d, 1H, J ¼ 16 Hz, –COCH), 3.45 (s, 3H,
–NCH3), 4.25 (d, 1H, J ¼ 9 Hz, –OCH), 4.78 (d, 1H, J ¼ 9 Hz, –OCH),
6.94–8.01 (m, 10H, ArH); 13C NMR (CDCl3, 125 MHz): dC ¼ 29.03
(NCH3), 42.24 (CH2CO), 48.77 (CH2C), 82.29 (OCH2), 114.62 (ArCH),
120.23 (ArC), 120.54 (ArCH), 120.98 (ArCH), 121.06 (ArCH), 122.38
(ArC), 122.97 (ArCH), 125.24 (ArCH), 125.99 (ArCH), 126.23 (ArCH),
127.39 (ArCH), 127.98 (ArCH), 130.21 (ArC), 134.11 (ArC), 139.21
(ArC), 155.51 (ArC), 167.31 (CO); MS: m/z ¼ 315 (Mþ); UV (EtOH):
lmax ¼ 234, 211 nm. Anal. calcd for C21H17NO2: C, 79.98; H, 5.43; N,
4.44. Found: C, 79.72; H, 5.73; N, 4.54.
Compound 5c. Yield: 95%; white solid; mp 120–1228C; IR (KBr): 2923,
1677, 1460, 758 cm21
;
1H NMR (CDCl3, 500 MHz): dH ¼ 2.94 (d, 1H,
J ¼ 16 Hz, –COCH), 3.40 (d, 1H, J ¼ 16 Hz, –COCH), 3.46 (s, 3H,
–NCH3), 4.34 (d, 1H, J ¼ 9 Hz, –OCH), 4.80 (d, 1H, J ¼ 9 Hz, –OCH),
6.94–7.87 (m, 10H, ArH); MS: m/z ¼ 315 (Mþ); UV (EtOH): lmax ¼ 240,
213 nm. Anal. calcd for C21H17NO2: C, 79.98; H, 5.43; N, 4.44. Found: C,
80.23; H, 5.58; N, 4.19.
Compound 5d. Yield: 92%; viscous liquid; IR (neat): 2920, 1679, 1479,
1
754 cm21; H NMR (CDCl3, 400 MHz): dH ¼ 2.22 (s, 3H, ArCH3), 2.25
(s, 3H, ArCH3), 2.85 (d, 1H, J ¼ 16 Hz, –COCH), 2.92 (d, 1H, J ¼ 16 Hz,
–COCH), 3.42 (s, 3H, –NCH3), 4.29 (d, 1H, J ¼ 9 Hz, –OCH), 4.51
(d, 1H, J ¼ 9 Hz, –OCH), 6.67–7.29 (m, 6H, ArH); MS: m/z ¼ 293 (Mþ);
UV (EtOH): lmax ¼ 286, 254, 217 nm. Anal. calcd for C19H19NO2: C,
77.79; H, 6.53; N, 4.77. Found: C, 78.09; H, 6.31; N, 4.88.
Compound 5e. Yield: 90%; viscous liquid; IR (neat): 2920, 1678, 1474,
1
755 cm21; H NMR (CDCl3, 400 MHz): dH ¼ 2.27 (s, 3H, ArCH3), 2.90
(d, 1H, J ¼ 16 Hz, –COCH), 2.96 (d, 1H, J ¼ 16 Hz, –COCH), 3.42