関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Lithium Chloride | HCID 433294 | — |
| 反応物 | Dimethyl [3-chloro-6-(methyloxy)-1,5-naphthyridin-4-yl]propanedioate | HCID 57707472 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Methyl [3-chloro-6-(methyloxy)-[1,5]naphthyridin-4-yl]acetate | HCID 57707490 | — |
反応手順
To a solution of dimethyl[3-chloro-6-(methyloxy)-1,5-naphthyridin-4-yl]propanedioate (56.23 g, 173 mmol) in DMSO (1210 ml) was added lithium chloride (14.9 g, 350 mmol) and water (3.24 ml, 180 mmol). The mixture was heated to 100° C. for 16 h then cooled and treated with ethyl acetate and water. The organic phase was washed twice with water, the aqueous extracted with ethyl acetate and this water-washed. The combined organic phases were dried and the solvent was removed. The residue was subjected to column chromatography on silica gel using a hexane and ethyl acetate gradient to provide the desired compound containing a little of the starting material (43.3 g, 94%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07732461B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-9a130c256b974de1a2dbc5a886740b40 |
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| 出典メモ | uspto-grants-2010_06 |
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