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【结 构 式】 
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【分子编号】22066 【品名】3,5-dichloro-4-[1,2-diamino-2-(2,6-dichloro-4-hydroxyphenyl)ethyl]phenol 【CA登记号】 |
【 分 子 式 】C14H12Cl4N2O2 【 分 子 量 】382.07236 【元素组成】C 44.01% H 3.17% Cl 37.12% N 7.33% O 8.38% |
合成路线1
该中间体在本合成路线中的序号：(I)The dichloroplatinum(II) complex (II) is synthesized by reacting K2PtCl4 with meso-1,2-bis(2,6-dichloro-4-hydroxyphenyl)ethylenediamine (I) in tert-BuOH / H2O or DMF / H2O at pH 5-6 and temperature below 40 C. The corresponding sulfatoplatinum(II) complex D-19384 is obtained by addition of Ag2SO4 to a suspension of the dichloro complex (II) in H20 at 40 C.
| 【1】 Schonenberger, H.; Von Argerer, E.; Karl, J.; Jennerwein, M.; Engel, J. (Asta Medica AG); Tumor inhibitor (1,2-diphenyl-ethylendiamine)-plat. DE 3604866; EP 0193055; ES 8707920; JP 1986194095; US 4730068 . |
| 【2】 Lux, F.; Hilgard, P.; Respondek, J.M.; Karl, J.; Engel, J.; Schonenberger, H.; Schumacher, W.; D-19384. Drugs Fut 1988, 13, 3, 215. |
合成路线2
该中间体在本合成路线中的序号：(I)meso-1,2-Bis(2,6-dichloro-4-hydroxyphenyl)ethylenediamine (I) is svnthesized by [3.3]sigmatropic diaza-Cope rearrangement according to the method of Vögtle and Goldschmitt by reaction of meso-1,2-bis(2-hydroxyphenyl)ethylenediamine (IV) with 2,6-dichloro-4methoxybenzaldehyde (V) at temperature below 120 C via the corresponding aldimine (VI) and subsequent ether cleavage with boron tribromide.
| 【1】 Vogtle, F.; Goldschmidt, E.; Chem Ber 1976, 109, 1. |
| 【2】 Lux, F.; Hilgard, P.; Respondek, J.M.; Karl, J.; Engel, J.; Schonenberger, H.; Schumacher, W.; D-19384. Drugs Fut 1988, 13, 3, 215. |
| 中间体序号 | 中间体编号 | 品名 | CAS号 | 分子式 | 供应商 | 用于合成 |
|---|---|---|---|---|---|---|
| (I) | 22066 | 3,5-dichloro-4-[1,2-diamino-2-(2,6-dichloro-4-hydroxyphenyl)ethyl]phenol | C14H12Cl4N2O2 | 详情 | 详情 | |
| (IV) | 22068 | 2-[1,2-diamino-2-(2-hydroxyphenyl)ethyl]phenol | C14H16N2O2 | 详情 | 详情 | |
| (V) | 22069 | 2,6-dichloro-4-methoxybenzaldehyde | C8H6Cl2O2 | 详情 | 详情 | |
| (VI) | 22070 | 2-[[(1,2-bis(2,6-dichloro-4-methoxyphenyl)-2-[[(E)-(2-hydroxyphenyl)methylidene]amino]ethyl)imino]methyl]phenol | C30H24Cl4N2O4 | 详情 | 详情 | |
| (VII) | 22071 | 2-[1,2-bis[[(E)-(2,6-dichloro-4-methoxyphenyl)methylidene]amino]-2-(2-hydroxyphenyl)ethyl]phenol | C30H24Cl4N2O4 | 详情 | 详情 | |
| (VIII) | 22072 | 1,2-bis(2,6-dichloro-4-methoxyphenyl)-1,2-ethanediamine; 2-amino-1,2-bis(2,6-dichloro-4-methoxyphenyl)ethylamine | C16H16Cl4N2O2 | 详情 | 详情 | |
| (IX) | 21351 | 2-Hydroxybenzaldehyde;Salicylic aldehyde；2-Formylphenol;salicylaldehyde | 90-02-8 | C7H6O2 | 详情 | 详情 |