, 6.68 (q, 2 H), 7.03 (s, 1 H), 7.13 (s, 2 H), 7.28?7.30 (m, 2 H). 13 C{ 1 H} NMR, vol.816, p.3380, 0907.
, + Calcd for C 38 H 59 N 2 S + , 575.4393; Found 575.4331. Characterization is in accordance with data reported in the literature, vol.40
, mmol) in water (48 mL) was added to a solution of freshly recrystallized 4?bromoaniline (1.04 g, 5.84 mmol) in CH 2 Cl 2 (12 mL). The mixture was stirred at r.t. for 4 h. The reaction mixture was extracted with CH, A solution of Oxone®, vol.2, p.400
, ? 7.78 (s, 4 H)
, bis(1?(4?bromophenyl)diazene) (20). to r.t., diluted with CH 2 Cl 2 (50 mL), washed with water (3 x 100 mL), dried over MgSO 4 , evaporated and purified by column chromatography (cyclohexane/ CH 2 Cl 2, p.26
, 1.71 (m, 6 H), vol.2
, 7.60 (d, 1 H), 7.65?7.67 (m, 4 H), 7.72?7.75 (d, 2 H), 7.79?7.82 (m, 4 H). 13 C{ 1 H} NMR
, olan?2?yl)phenyl)diazene) (AB?3HT?(BPin) 2 ) (21)
, After cooling down to r.t. the reaction mixture was diluted with CH 2 Cl 2 (100 mL), filtered over celite to remove the Pd catalyst, washed with brine (2 x 100 mL) and H 2 O (3 x 100 mL
, Signals for the two carbon atoms attached to boron atoms are missing due to quadrupolar relaxation. 11 B NMR (CDCl 3 , 128 MHz): ? 29.3 (s). FTIR (UATR) ? (cm -1 ): 2923, 2853, 73?7.76 (m, 2 H), 7.89?7.92 (m, 4 H), 7.96?7.99 (m, 4 H). 13 C{ 1 H} NMR
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