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Tetrahydrofuran → 2-(N-methoxymethylanilino)-4-methyl-6-(1-propynyl)pyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Mepanipyrim | HCID 86296 | — |
| 生成物 | 2-(N-methoxymethylanilino)-4-methyl-6-(1-propynyl)pyrimidine | HCID 14327558 | 63% |
反応手順
2-Anilino-4-methyl-6-(1-propynyl)pyrimidine (2.2 g) was added to a suspension in 50 ml of tetrahydrofuran of 0.5 g of sodium hydride (60%) of which oily component was removed with n-hexane, and the mixture was stirred for 30 minutes at 50°-55° C. After cooling to room temperature, 1.0 g of chloromethyl methyl ether was added to the mixture and stirred for 3 hours. The reaction mixture was poured into water and extracted with 150 ml of toluene. the toluene layer was washed with water, dried over Glauber's salt and concentrated by evaporation under reduced pressure. The residue was purified by silica gel column chromatography to obtain 1.7 g (yield: 63%) of 2-(N-methoxymethylanilino)-4-methyl-6-(1-propynyl)pyrimidine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04992438 |
| 出典データセット | uspto-grants-1991_02 |
| ORD ID | ord-a7caa4a59af64945bc3a477998e00b03 |
| 出典メモ | uspto-grants-1991_02 |