97人妻一区二区精品免费,好男人社区www在线官网,办公室娇喘的短裙老师在线视频,亚州精品久久久久久久久

將0.4 mL三氯氧磷滴加到由0.4 mL 3, 3-二甲氨基丙烯醛和4 mL二氯甲烷組成的混合溶液, 在0 ℃下攪拌15 min.然后在相同溫度下, 攪拌加入到已經(jīng)預(yù)冷至－5 ℃的含有128 mg鋅配合物5(0.184 mmol)的20 mL二氯甲烷中.撤去冰水浴, 室溫?cái)嚢?8 h.攪拌下加入120 mL飽和碳酸氫鈉水溶液, 室溫?cái)嚢柽^夜, 用二氯甲烷萃取反應(yīng)液(30 mL×3), 合并有機(jī)層并水洗兩次, 無(wú)水硫酸鈉干燥后用重氮甲烷進(jìn)行甲基化處理, 減壓除去溶劑, 將所得固體混合物用硅膠柱層析分離[洗脫劑: V(石油醚):V(乙酸乙酯)＝3:1], 得75 mg紅色固體6 (0.108 mmol), 產(chǎn)率59%. m.p. 206~209 ℃; UV-vis (CH₂Cl₂)λ_max [ε/(L?mol^－1?cm^－1)]: 367 (5.93×10³), 420 (1.12×10⁴), 532 (9.41×10²), 570 (5.08×10³), 735 (9.45×10³) nm; ¹H NMR (CDCl₃) δ: －0.02 (br s, 1H, NH), 0.60 (br s, 1H, NH), 0.88 (t, J＝6.6 Hz, N-C-C-C-CH₃), 1.30 (t, J＝7.6 Hz, 3H, 8a-CH₃), 1.63 (d, J＝7.2 Hz, 3H, 18-CH₃), 1.18~1.78 (m, 4H, NC-CH₂CH₂-C), 1.98~2.20 (m, 2H, 17a+17b-H), 2.27~2.50 (m, 1H, 17a+17b-H), 2.76~2.87 (m, 1H, 17a+17b-H), 2.98, 3.09, 3.62, 3.72 (each s, each 3H, CH₃+OCH₃), 3.56 (q, J＝7.6 Hz, 2H, 8a-H), 4.34 (t, J＝6.6 Hz, 2H, NCH₂-), 4.61 (q, J＝7.2 Hz, 1H, 18-H), 5.11 (dd, J＝8.8, 2.7 Hz, 1H, 17-H), 6.12 (d, J＝17.8 Hz, 1H, trans-3b-H), 6.16 (d, J＝11.5 Hz, 1H, cis-3b-H), 6.19 (dd, J＝15.7, 7.7 Hz, 1H, 20b-H), 7.71 (dd, J＝17.8, 11.5 Hz, 1H, 3a-H), 8.93 (d, J＝15.7 Hz, 1H, 20a-H), 9.30, 9.36 (each s, each 1H, meso-H), 10.11 (d, J＝7.7 Hz, 20b-CHO); ¹³C NMR (CDCl₃) δ: 201.1, 174.4, 172.8, 166.0, 161.7, 154.0, 151.3, 146.7, 144.7, 143.6, 140.7, 139.6, 137.1, 136.2, 135.7, 133.8, 131.0, 130.7, 130.2, 129.9, 123.2, 106.6, 106, 1, 101.8, 94.0, 52.6, 52.2, 49.8, 31.7, 31.2, 31.0, 30.7, 30.6, 26.1, 24.4, 24.3, 20.0, 18.2, 12.9, 12.8, .11.8; IR (KBr) v: 3346 (N—H), 2960 (C—H), 1738, 1704 (C＝O), 1664 (C＝C), 1542 (chlorin skeleton), 1458, 1365, 1174, 1068, 981 cm^－1; EI-MS m/z: 688.2 (M+H⁺). Anal. calcd for C₄₁H₄₅N₅O₅: C 71.59, H 6.59, N 10.18; found C 71.61, H 6.44, N 9.99.