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Triethylamine → methanesulfonic acid 2-{2-[4-(4,5-Dichloro-2-fluoro-phenylamino)-6-nitro-quinazolin-7-yloxy]-ethoxy}-ethyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 2-{2-[4-(4,5-Dichloro-2-fluoro-phenylamino)-6-nitro-quinazoline-7-yloxy]-ethoxy}-ethanol | HCID 69266955 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | methanesulfonic acid 2-{2-[4-(4,5-Dichloro-2-fluoro-phenylamino)-6-nitro-quinazolin-7-yloxy]-ethoxy}-ethyl ester | HCID 86618842 | 101.9% |
反応手順
Compound 29a (0.035 gram, 0.076 mmol) was dissolved in dichloromethane (4.3 ml) and triethylamine (0.032 gram, 3.82 mmol) was added to the resulting solution. Methanesulfonyl chloride (MsCl, 0.025 gram, 0.022 mmol) was then added and the resulting mixture was stirred at room temperature for 3 hours. The mixture was thereafter extracted twice with CH2Cl2, washed with brine and dried over sodium sulfate. The crude residue was purified by silica gel column chromatography, using a mixture of 2% methanol in dichloromethane as eluent, to give Compound 32a (0.012 gram, 29% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08461166B2 |
| 出典データセット | uspto-grants-2013_06 |
| ORD ID | ord-b82539dee92c4eb18b087b6a469bbbd4 |
| 出典メモ | uspto-grants-2013_06 |