在50 mL二氯甲烷和25 mL甲醇混合液中溶解187 mg MPPb (1c, 0.301 mmol), 在0℃下将溶解于30 mL甲醇的150 mg三水硝酸铊(III)迅速加入到反应液中, 并在此温度下搅拌反应15 min, 然后加入30 mL亚硫酸氢钠甲醇饱和溶液, 室温搅拌20 min后滴加2 mL浓盐酸进行酸化, 将所产生的大量白色沉淀过滤, 分出有机层, 水层用二氯甲烷萃取(20 mL×3), 合并有机层并水洗一次, 用无水硫酸钠干燥后减压浓缩至干, 剩余物经硅胶柱层析[洗脱剂: V(石油醚):V(乙酸乙酯)＝4:1], 得到148 mg黑绿色固体9 (0.217 mmol), 产率72%. mp. 197~199 ℃; UV-vis (CH2Cl2)λmax [ε/(L?mol－1?cm－1)]: 418 (1.12×105), 484 (2.85×103), 512 (1.02×103), 552 (1.09×104), 666 (3.72×104) nm; 1H NMR (CDCl3) δ: －1.49 (br s, 1H, NH), 0.64 (br s, 1H, NH), 1.83 (t, J＝7.6 Hz, 3H, 8-CH3), 1.81 (d, J＝7.2 Hz, 3H, 18-CH3), 2.17~2.33 (m, 2H, 17a+17b-H), 2.46~2.88 (m, 2H, 17a+17b-H), 3.31, 3.53 (6H), 3.59, 3.67, 3.90 (each s, all 18H, CH3+OCH3), 4.05 (q, J＝7.6 Hz, 2H, 8a-H), 4.11 (d, J＝5.0 Hz, 2H, 3a-H), 4.18 (d, J＝8.0 Hz, 1H, 17-H), 4.44 (q, J＝7.0 Hz, 1H, 18-H), 5.09 (t, J＝5.0 Hz, 1H, 3b-H), 6.22 (s, 1H, 132-H), 8.53, 9.56, 10.25 (each s, each 1H, meso-H), 11.15 (s, 1H, 7-CHO); IR (KBr) v: 3333 (N—H), 2851 (C—H), 1733, 1708 (C＝O), 1614 (C＝C), 1565 (chlorin skeleton), 1490, 1440, 1260, 1146, 1083, 1006 cm－1; EI-MS m/z: 683.4 (M+H+). Anal. calcd for C38H42N4O8: C 66.85, H 6.20, N 8.21; found C 66.71, H 6.47, N 8.35.

化学慧定制合成事业部