関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloromethyl Methyl Ether | HCID 7864 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 3-Hydroxyphthalic anhydride | HCID 96580 | — |
| 溶媒 | 1,1-Dichloroethane | HCID 6365 | — |
| 生成物 | 3-Methoxymethyloxyphthalic anhydride | HCID 21936735 | 99.2% |
反応手順
N,N-Diisopropylethylamine (4.39 g, 34.0 mmol) was added to a solution of 3-hydroxyphthalic anhydride (5.0 g, 30.5 mmol) in dichloroethane (60 ml), then chloromethyl methyl ether (2.57 g, 32.0 mmol) was dropped thereinto under cooling with ice water and the mixture was returned to room temperature and stirred for 1 hour. Then N,N-diisopropylethylamine (2.20 g, 17.0 mmol) and chloromethyl methyl ether (1.28 g, 16.0 mmol) were further added thereto followed by stirring for 1 hour. After the reaction, the solvent was evaporated and the residue was diluted with water followed by extracting with ether. The organic layer was washed with water and a saturated sodium chloride solution successively and dried over anhydrous magnesium sulfate and the solvent was evaporated therefrom to provide 6.3 g (yield 99%) of 3-methoxymethyloxyphthalic anhydride as colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06969711B2 |
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| 出典データセット | uspto-grants-2005_11 |
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| ORD ID | ord-467e662847c44e3ea5003641010b370c |
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| 出典メモ | uspto-grants-2005_11 |
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