HRID731045

反应详情

EQUATION

反应方程式

HRID 731045 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The desired product was prepared using a procedure similar to step 6 of example 3. Thus, [4-(9-benzyl-6,7,8,9-tetrahydro-5H-carbazol-3-yl)-phenoxy]-acetonitrile (0.357 g, 0.910 mmol) was reacted with NaN3 (0.296 g, 4.548 mmol) and NH4Cl (0.243 g, 4.548 mmol) in DMF (10 ml) to give the product (0.329 g, 0.755 mmol, 83%) as a white solid, dec. 228-230° C. 1H NMR (DMSO-d6) δ 1.79-1.85 (m, 4H), 2.64-2.71 (m, 4H), 5.33 (s, 2H), 5.50 (s, 2H), 7.03 (d, J=7.6 Hz, 2H), 7.11 (d, J=8.7 Hz, 2H), 7.21 (t, J=7.2 Hz, 1H), 7.27-7.30 (m, 3H), 7.39 (d, J=8.6 Hz, 1H), 7.59-7.61 (m, 3H), 16.80 (broad s, 1H); IR (solid) 3030, 2920, 2590, 1520, 1470 and 1240 cm−1; [ESI(+)], m/z 436 (M+H)+; Anal. Calcd. for C27H25N5O: C, 74.46; H, 5.79; N, 16.08; Found: C, 74.34; H, 5.46; N, 16.26.