COMMUNICATIONS
Pragati K Prasad and Arumugam Sudalai
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1723, 2918, 3077 ; H NMR (200 MHz, CDCl3): d=2.45–2.72
analysis: C9H6O2 requires C 73.97, H 4.14, O 21.89; found:
C 73.94, H 4.17, O 21.89%.
(m, 2H) 2.87–3.07 (m, 2H) 4.51–4.62 (m, 1H), 5.13–5.24 (m,
2H), 5.79–5.97 (m, 1H) 7.21–7.56 (m, 3H), 8.07 (dd, J=0.8
and 7.7 Hz, 1H); 13C NMR (125 MHz,) CDCl3: d=32.5,
39.2, 77.6, 118.8, 125.2, 127.3, 127.6, 130.3, 132.3, 133.6,
138.9, 164.9; HR-MS (ESI+): m/z=211.0730, calcd. for
(C12H12O2)+ [(M+Na)+]: 211.0727; analysis: C12H12O2 re-
quires C 76.57, H 6.43, O 17.00; found: C 76.58, H 6.33, O
17.09%.
2H-Chromen-2-one (3r): Yield: 0.355 g (2.430 mmol,
81%); colorless liquid; IR (CHCl3): umax =820, 1104, 1180,
1
1610, 1710, 3030 cmÀ1; H NMR (200 MHz, CDCl3): d=6.43
(d, J=9.4 Hz, 1H), 7.28–7.57 (m, 4H), 7.77 (d, J=9.4 Hz,
1H); 13C NMR (50 MHz, CDCl3) d 116.7, 116.9, 118.8,
124.4, 127.8, 131.8, 143.5, 154.0, 160.8; analysis: C9H6O2 re-
quires C 73.97, H 4.14, O 21.89; found: C 73.94, H 4.17, O
21.89%.
3-Allyl-7-methylisochroman-1-one (3m): Yield: 0.521 g
(2.579 mmol, 86%); colorless oil; IR (CHCl3): umax =774,
3-Allyl-5-fluoroisobenzofuran-1(3H)-one
(3s):
Yield:
921, 1082, 1194, 1723, 2923, 3078 cmÀ1; H NMR (200 MHz,
0.530 g (2.760 mmol, 92%); colorless oil; IR (CHCl3): umax
=
1
1
CDCl3): d=2.39 (s, 3H), 2.51–2.68 (m, 2H), 2.82–2.94 (m,
2H), 4.48–4.61 (m, 1H), 5.12–5.23 (m, 2H), 5.77–6.00 (m,
1H) 7.10 (d, J=7.7 Hz, 1H) 7.32 (d, J=7.7 Hz, 1H), 7.90 (s,
1H); 13C NMR (50 MHz, CDCl3): d=20.9, 32.1, 39.2, 77.7,
118.7, 124.8, 127.2, 130.4, 132.4, 134.4, 135.9, 137.3, 165.2;
HR-MS (ESI+): m/z=225.0886, calcd. for (C13H14O2)+ [(M+
Na)+]: 225.0884; analysis: C13H14O2 requires C 77.20, H 6.98,
O 15.82; found: C 77.38, H 6.83, O 15.79%.
988, 1100, 1247, 1483, 1604, 1624, 1766, 3100 cmÀ1; H NMR
(200 MHz, CDCl3): d=2.62–2.78 (m, 2H), 5.12–5.25 (m,
2H), 5.48 (t, J=6.1 Hz, 1H), 5.65–5.86 (m, 1H), 7.12–7.28
(m, 2H), 7.89 (dd, J=4.8 and 8.1 Hz, 1H); 13C NMR
(50 MHz, CDCl3): d=38.2, 79.2, 109.3, 117.2, 119.8, 122.2,
127.8, 130.6, 151.9, 163.6, 168.7; analysis: C11H9FO2 requires
C 68.75, H 4.72, F 9.89, O 16.65; found: C 68.82, H 4.97, O,
26.21%.
3-Allyl-6-methoxyisochroman-1-one (3n): Yield: 0.569 g
(2.610 mmol, 87%); colorless oil; IR (CHCl3): umax =778,
3-Allyl-5-methoxyisobenzofuran-1(3H)-one (3t): Yield:
0.518 g (2.551 mmol, 85%); colorless oil; IR (CHCl3): umax
=
917, 1027, 1260, 1606, 1716, 2920, 3076 cmÀ1
;
1H NMR
692, 1073, 1103, 1259, 1605, 1744, 2997 cmÀ1 1H NMR
;
(200 MHz, CDCl3): d=2.48–3.04 (m, 4H), 3.86 (s, 3H),
4.49–4.60 (m, 1H), 5.16–5.24 (m, 2H), 5.83–6.00 (m, 1H),
6.70 (d, J=2.4 Hz, 1H), 6.87 (dd, J=2.4 and 8.3 Hz, 1H),
8.02 (d, J=8.3 Hz, 1H); 13C NMR (50 MHz, CDCl3): d=
32.7, 39.1, 55.4, 77.4, 112.0 113.4, 117.5, 118.7, 132.3, 132.4,
141.2, 163.7, 165.3; HR-MS (ESI+): m/z=241.0835, calcd.
for (C13H14O3)+ [(M+Na)+]: 241.0831; analysis: C13H14O3 re-
quires C 71.54, H 6.47, O 21.99; found: C 71.58, H 6.53, O
21.89%.
(200 MHz, CDCl3): d=2.56–2.81 (m, 2H), 3.91 (s, 3H),
5.15–5.25 (m, 2H), 5.42 (t, J=6.1 Hz, 1H), 5.68- 5.89 (m,
1H), 6.87 (d, J=1.6 Hz, 1H), 7.02 (dd, J=1.6 and 8.5 Hz,
1H), 7.80 (d, J=8.5 Hz, 1H); 13C NMR (50 MHz, CDCl3):
d=38.8, 55.7, 79.3, 106.1, 116.2, 118.7, 119.6, 127.2, 131.3,
152.0, 164.5, 169.8; analysis: C12H12O3 requires C 70.58, H
5.92, O 23.50; found: C 70.61, H 5.67, O 23.72%.
5-Bromoisobenzofuran-1(3H)-one (3u): Yield: 0.498 g
(2.338 mmol (78%); colorless solid; mp 1628C; 1H NMR
(200 MHz, CDCl3): d=5.30 (s, 2H), 7.68 (t, J=3.7 Hz, 2H),
7.77–7.81 (m, 1H); 13C NMR (50 MHz, CDCl3): d=68.8,
124.9, 125.6, 127.1, 129.2, 132.7, 148.2, 169.7; analysis:
C8H5BrO2 requires C 45.11, H 2.37, Br 37.51, O 15.02;
found: C 45.65, H 2.24, Br 38.13, O 13.98%.
3-Allyl-6-fluoroisochroman-1-one (3o): Yield: 0.536 g
(2.640 mmol, 88%); colorless oil; IR (CHCl3): umax =667,
755, 1107, 1267, 1615, 1725, 2919, 3079 cmÀ1 1H NMR
;
(200 MHz, CDCl3): d=2.45–2.72 (m, 2H) 2.84–3.08 (m,
2H), 4.51- 4.65 (m, 1H), 5.16–5.25 (m, 2H), 5.78–5.99 (m,
1H), 6.93 (dd, J=2.3 and 8.1 Hz, 1H), 7.06 (dt, J=2.3 and
8.1 Hz, 1H), 8.10 (dd, J=5.6 and 8.6 Hz, 1H); 13C NMR
(125 MHz, CDCl3): d=32.6, 39.1, 77.5, 114.3, 115.3, 119.1,
121.5, 132.1, 133.3, 141.9, 164.0, 166.8; HR-MS (ESI+):
m/z=229.0635, calcd. for (C12H11O2F)+ [(M+Na)+]:
229.0632; analysis: C12H11O2F requires C 69.89, H 5.38, F
9.21, O 15.52; found: C 69.95, H 5.54, F 9.13, O 15.38%.
3-Heptylisobenzofuran-1(3H)-one (3v): Yield: 0.633 g
(2.728 mmol, 91%); colorless oil; 1H NMR (200 MHz,
CDCl3): d=0.88 (t, J=3.5 Hz, 3H), 1.27–1.47 (m, 10H),
1.66–1.82 (m, 1H), 1.96–2.12 (m, 1H), 5.46 (dd, J=4.0 and
7.4 Hz, 1H), 7.41–7.55 (m, 2H), 7.66 (dt, J=1.6 and 7.6 Hz,
1H). 7.88 (d, J=7.6 Hz, 1H); 13C NMR (50 MHz, CDCl3):
d=14.0, 22.5, 24.8, 29.0, 29.3, 31.7, 34.7, 81.2, 121.6, 125.6,
126.2 128.9, 133.8, 150.0, 170.3; analysis: C15H20O2 requires
C 77.55, H 8.68, O 13.77; found: C 77.58, H 8.71, O 13.71%.
3-Butylisobenzofuran-1(3H)-one (3w): Yield: 0.496 g
(2.610 mmol, 87%); colorless oil; 1H NMR (200 MHz,
CDCl3): d=0.91 (t, J=6.3 Hz, 3H), 1.26–1.52 (m, 4H),
1.71–1.82 (m, 1H), 1.98–2.12 (m, 1H), 5.46 (dd, J=4.1 and
7.2 Hz, 1H), 7.50 (dd, J=7.2 and 9.8 Hz, 2H), 7.67 (t, J=
7.2 Hz, 1H), 7.88 (d, J=7.8 Hz, 1H); 13C NMR (50 MHz,
CDCl3): d=13.8, 22.4, 26.8, 34.4, 81.1, 121.6, 125.6, 126.2,
128.9, 133.8,150.0, 170.2; analysis: C12H14O2 requires C
75.76, H 7.42, O 16.82; found: C 75.54, H 7.57, O 16.89%.
Isobenzofuran-1,3-dione (3x): Yield: 0.426 g (2.878 mmol,
96%); colorless solid; mp 1318C; IR (CHCl3): umax =667,
6,7,8-Trimethoxy-1-oxoisochromane-5-carbonitrile
(3p):
Yield: 0.663 g (2.520 mmol, 84%); yellowish solid; mp
1078C; IR (CHCl3): umax =802, 1036, 1130, 1579, 1677, 1713,
2922, 2949 cmÀ1 1H NMR (200 MHz, CDCl3): d=3.31 (t,
;
J=8.5 Hz, 2H), 3.85 (s, 3H), 3.95 (s, 3H), 4.04 (s, 3H), 4.65
(t, J=8.5 Hz, 2H); 13C NMR (125 MHz, CDCl3): d=27.4,
61.4, 61.8, 62.2, 65.7, 100.3, 113.8, 115.2, 141.2, 145.1, 159.6,
159.7, 161.2; HR-MS (ESI+): m/z=286.0693, calcd. for
(C13H13NO5)+ [(M+Na)+]: 286.0691; analysis: C13H13NO5 re-
quires C 59.31, H 4.98, N 5.32, O 30.39; found: C 58.95, H
4.57, N 5.27, O 31.21%.
6-Allyl-5,6-dihydro-8H-pyranoACTHNUGTRNEUNG[3,4-b]pyridin-8-one (3q):
Yield: 0.476 g (2.518 mmol, 84%); yellow oil; 1H NMR
(200 MHz, CDCl3): d=2.29–2.73 (m, 4H), 5.05–5.19 (m,
2H), 5.23 (s, 1H), 5.79–5.96 (m, 1H), 7.27 (dd, J=4.9 and
7.6 Hz, 1H), 7.92 (dd, J=1.5 Hz and 7.6 Hz, 1H), 8.28 (dd,
J=1.5 and 4.9 Hz, 1H); 13C NMR (125 MHz, CDCl3): d=
40.4, 42.0, 69.3, 118.9, 122.4, 133.3, 134.0, 140.4, 147.7, 151.5;
758, 1052, 1307, 1604, 1748, 1772, 2924 cmÀ1 1H NMR
;
(200 MHz, CDCl3): d=7.77 (dd, J=2.0 and 6.0 Hz, 2H),
7.89 (dd, J=2.0 and 6.0 Hz, 2H); 13C NMR (100 MHz,
CDCl3): d=123.6, 132.7, 134.3, 167.7; HR-MS (ESI+): m/z=
149.0233, calcd. for (C8H5O3)+: 149.0232; analysis: C8H4O3
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ꢀ 2014 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim
Adv. Synth. Catal. 0000, 000, 0 – 0
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