化工社化工社 化学情報印刷レポート · 研究参考用
Methanesulfonic Acid → N-Desmethyl imatinib mesylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanesulfonic Acid | HCID 6395 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Cgp-74588 | HCID 9869737 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | N-Desmethyl imatinib mesylate | HCID 10188302 | — |
反応手順
4.8 g (10 mmol) of N-[4-methyl-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-phenyl]-4-piperazin-1-ylmethyl-benzamide are dissolved in 20 ml of ethanol under heating and 0.99 g of methanesulfonic acid are added. After addition of ethyl acetate the product cristallizes. Drying at 50 mbar and 60° C. yields N-[4-methyl-3-(4-pyridin-3-yl-pyrimidin-2-ylamino)-phenyl]-4-piperazin-1-ylmethyl-benzamide methanesulfonate; Rf=0.17 (methylene chloride:ethyl acetate:methanol:conc. aqueous ammonium hydroxide solution=60:10:30:2); tR (HPLC)2) 14.6 min; m.p. 242-245° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07312216B2 |
| 出典データセット | uspto-grants-2007_12 |
| ORD ID | ord-08b49c26df48452d8d881cedddbfd239 |
| 出典メモ | uspto-grants-2007_12 |