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Methyl chloroformate → 1-Methoxycarbonyloxy-2,4-dimethoxynaphthalene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl chloroformate | HCID 6586 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Hydroxy-2,4-dimethoxynaphthalene | HCID 12563547 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Methoxycarbonyloxy-2,4-dimethoxynaphthalene | HCID 14183043 | — |
反応手順
To a solution of 1.27 g of 1-hydroxy-2,4-dimethoxynaphthalene, prepared as shown in Preparations 7 and 8, in 50 ml of tetrahydrofuran was added 0.694 g of methyl chloroformate followed by 0.743 g of triethylamine. The mixture was stirred at room temperature for 16 hours, filtered, then the solvent removed under reduced pressure. The residue was dissolved in diethyl ether, washed with dilute hydrochloric acid and dried over anhydrous sodium sulfate. The ether was removed under reduced pressure and the residue chromatographed on silica gel, eluting with a 1:1 mixture of methylene chloride and hexane, to give 1-methoxycarbonyloxy-2,4-dimethoxynaphthalene, m.p. 128°-129° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05155132 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-51a4826d03fb4eae92e228d814dc4a1d |
| 出典メモ | uspto-grants-1992_10 |