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N,N,N',N'-Tetramethylazodicarboxamide → 2-(3-{2-[2-(4-Chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-ethoxy}-phenoxy)-2-methyl-propionic acid ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N,N',N'-Tetramethylazodicarboxamide | HCID 4278 | — |
| 反応物 | Tributylphosphine | HCID 13831 | — |
| 反応物 | Ethyl 2-(3-hydroxyphenoxy)-2-methylpropanoate | HCID 46835528 | — |
| 反応物 | 2-[2-(4-Chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-ethanol | HCID 66619310 | — |
| 生成物 | 2-(3-{2-[2-(4-Chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-ethoxy}-phenoxy)-2-methyl-propionic acid ethyl ester | HCID 66619219 | — |
反応手順
The title compound was prepared in analogy to Example 4, intermediate, from 2-[2-(4-chloro-phenyl)-5,6-difluoro-benzoimidazol-1-yl]-2-cyclohexyl-ethanol (Ex. 1, int. c), 2-(3-hydroxy-phenoxy)-2-methyl-propionic acid ethyl ester (CAS RN: 328919-24-0), tri-n-butylphosphin and N,N,N′,N′-tetramethylazodicarboxamide. The compound was purified by silica gel chromatography using a MPLC system (CombiFlash Companion, Isco Inc.) eluting with a gradient of n-heptane:ethyl acetate (100:0 to 70:30). Light yellow solid (19%). MS (Turbo Spray): m/z=597.2 [M+H].
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08088930B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-309084d44c8d492580770f3b344db576 |
| 出典メモ | uspto-grants-2012_01 |