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Diisopropylcarbodiimide → (4-{1-(4-Fluorophenyl)-3-[3-(4-fluorophenyl)-3-hydroxypropyl]-4-oxoazetidin-2-yl}benzylcarbamoyl)methanesulfonic Acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylcarbodiimide | HCID 12734 | — |
| 反応物 | Sulfoacetic acid | HCID 31257 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 4-(4-Aminomethylphenyl)-1-(4-fluorophenyl)-3-[3-(4-fluorophenyl)-3-hydroxypropyl]azetidin-2-one | HCID 22252032 | — |
| 反応物 | HCID 178418300 | HCID 178418300 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (4-{1-(4-Fluorophenyl)-3-[3-(4-fluorophenyl)-3-hydroxypropyl]-4-oxoazetidin-2-yl}benzylcarbamoyl)methanesulfonic Acid | HCID 21083138 | — |
反応手順
A solution of 120 mg of 4-(4-aminomethylphenyl)-1-(4-fluorophenyl)-3-[3-(4-fluorophenyl)-3-hydroxypropyl]azetidin-2-one (17), and 48 μl of diisopropylethylamine in 1 ml of dimethylformamide was added to a solution of 40 mg of sulfoacetic acid, 110 μl of diisopropylcarbodiimide, and 76 mg of hydroxybenzotriazole in 2 ml of dimethylformamide, and the mixture was stirred at room temperature for 12 h. The reaction solution was concentrated and separated by HPLC (Knauer Eurospher-100-10-C18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20->10/90). This gave the product of molecular weight 544.58 (C27H26F2N2O6S1); MS (ESI) 527.10 (M+H+—H2O)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07176193B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-3e2da4d0ec654069983200b41eadd3b8 |
| 出典メモ | uspto-grants-2007_02 |