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【结 构 式】 
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【分子编号】44613 【品名】 【CA登记号】 |
【 分 子 式 】C6H7Cl2N 【 分 子 量 】164.03372 【元素组成】C 43.93% H 4.3% Cl 43.23% N 8.54% |
合成路线1
该中间体在本合成路线中的序号：(IV)A synthesis for [benzene-U-14C]-tiludronate has been described: The chlorination of [U-14C]-acetanilide (I) with tetrabutylammonium iodotetrachloride gives the corresponding 4-chloro derivative (II) (along with some of the 2-chloro isomer). The hydrolysis of (II) with concentrated HCl at 60 C yields the chloroaniline (III), which is converted to the corresponding diazonium salt (IV) with NaNO2 and HCl. The reaction of (IV) with ferric thiocyanate affords the labeled 4-chlorophenylthiocyanate (V), which is condensed with the lithium salt of methylenebis(phosphonic acid)tetraisopropyl ester (VI) in THF to yield 4-chlorophenylsulfanylmethylenebis(phosphonic acid)tetraisopropyl ester (VII). Finally, this compound is hydrolyzed with concentrated HCl or aqueous NaOH.
| 【1】 Ellames, G.J.; Burgos, A.; Synthesis of disodium [benzene-U-C-14]-(4-chlorophenylthio)methylene diphosphonate, [benzene-U-C-14]-tiludronate. J Label Compd Radiopharm 1995, 36, 11, 1071. |
| 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) | 10194 | N-Phenylacetamide; Acetanilide | 103-84-4 | C8H9NO | 详情 | 详情 |
| (I) | 44610 | C8H9NO | 详情 | 详情 | ||
| (II) | 10195 | N-(4-Chlorophenyl)acetamide | 539-03-7 | C8H8ClNO | 详情 | 详情 |
| (II) | 44611 | C8H8ClNO | 详情 | 详情 | ||
| (III) | 10196 | 4-Chlorobenzenaminium chloride | C6H7Cl2N | 详情 | 详情 | |
| (III) | 44612 | C6H7Cl2N | 详情 | 详情 | ||
| (IV) | 10197 | 4-Chlorobenzenediazonium chloride | C6H4Cl2N2 | 详情 | 详情 | |
| (IV) | 44613 | C6H7Cl2N | 详情 | 详情 | ||
| (V) | 10198 | 4-Chlorophenyl thiocyanate | 3226-37-7 | C7H4ClNS | 详情 | 详情 |
| (V) | 44614 | C7H4ClNS | 详情 | 详情 | ||
| (VI) | 10199 | [Bis(diisopropoxyphosphoryl)methyl]lithium | C13H29LiO6P2 | 详情 | 详情 | |
| (VII) | 10200 | Diisopropyl [(4-chlorophenyl)sulfanyl](diisopropoxyphosphoryl)methylphosphonate | C19H33ClO6P2S | 详情 | 详情 | |
| (VII) | 44615 | C19H33ClO6P2S | 详情 | 详情 |