CC(N=NC(C#N)(C)C)(C#N)C.C1C(=O)N(Br)C(=O)C1.[I:21][C:22]1[C:30]2[O:29][CH2:28][CH2:27][C:26]=2[CH:25]=[C:24]([S:31]([Cl:34])(=[O:33])=[O:32])[CH:23]=1.C(#N)C>ClC1C=CC=CC=1>[I:21][C:22]1[C:30]2[O:29][CH:28]=[CH:27][C:26]=2[CH:25]=[C:24]([S:31]([Cl:34])(=[O:32])=[O:33])[CH:23]=1
AIBN (270 mg, 1.3 mmol) and NBS (2.5 g, 14 mmol) were added to 7-iodo-2,3-dihydro-benzofuran-5-sulfonyl chloride (4.4 g, 13 mmol; Intermediate 55) in chlorobenzene (30 mL) at 70° C. The heating was turned off one hour after the addition. Acetonitrile (30 mL) was added and the organic phase was washed with sodium sulphite in water. The organic phase was separated and the volatiles were evaporated to give 4 g (90%) of the title compound as yellow crystals. 1H NMR 270 MHz (CDCl3) δ ppm 7.07 (d, J=2.23 Hz, 1H) 7.90 (d, J=2.23 Hz, 1H) 8.29-8.37 (m, 1H).
Wird geladen…
