将46 mg二氢卟吩镍配合物3 (0.071 mmol)溶解于6 mL浓硫酸中, 室温搅拌反应2 h, 用20%饱和的碳酸氢钠将所形成的反应溶液中和至pH约等于2, 加入100 mL二氯甲烷分层, 水洗有机层(100 mL×2), 用无水硫酸钠干燥后再经重氮甲烷甲基化, 浓缩后用硅胶柱层析分离[洗脱剂: V(石油醚):V(乙酸乙酯)＝5:1], 得19 mg黑色固体4(0.031 mmol), 产率44%. m.p. 192~195 ℃; UV-vis (CH₂Cl₂)λ_max [ε/(L•mol^－1•cm^－1)]: 409 (1.58×10⁴), 541 (9.28×10²), 588 (8.27×10²), 618 (7.11×10²), 690 (1.23×10⁴) nm; ¹H NMR (CDCl₃) δ: 0.04 (br s, 1H, NH), 0.13 (br s, 1H, NH), 1.70 (t, J＝7.6 Hz, 3H, 8-CH₃), 1.83 (d, J＝7.0 Hz, 3H, 18-CH₃), 1.95~2.08 (m, 1H, 17a+17b-H), 2.28~2.42 (m, 2H, 17a+17b-H), 2.53~2.72 (m, 2H, 17a+17b-H), 2.28, 3.21, 3.59, 3.61, 4.22 (each s, each 3H, CH₃+OCH₃), 3.69 (q, J＝7.6 Hz, 2H, 8a-H), 4.43 (q, J＝7.2 Hz, 1H, 18-H), 5.07 (d, J＝10.1 Hz, 1H, 17-H), 5.18 (d, J＝11.2 Hz, 1H, cis-3b-H), 6.32 (d, J＝17.6 Hz, 1H, trans-3b-H), 7.95 (dd, J＝17.6, 11.2 Hz, 1H, 3b-H), 8.56, 9.40, 9.62 (each s, each 1H, meso-H), 11.49 (s, 1H, 20-CHO); IR (KBr) ν: 3455 (N—H), 2958, 2867 (C—H), 1743, 1725 (C＝O), 1642 (C＝C), 1532 (chlorin skeleton), 1441, 1310, 1150, 104 cm^－1; EI-MS m/z: 595.4 (MH⁺). Anal. calcd for C₃₅H₃₈N₄O₅: C 70.69, H 6.44, N 9.42; found C 70.59, H 6.37, N 9.31.

化学慧定制合成事业部