関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methyl isopropenyl ketone | HCID 13143 | — |
| 反応物 | Dimethyl methoxymalonate | HCID 78718 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | Methyl 2-hydroxy-1-methoxy-5-methyl-4-oxocyclohex-2-enecarboxylate | HCID 18755506 | — |
反応手順
A 30% solution of 35.8 g of sodium methoxide is introduced into 65 ml of dimethyl sulfoxide and, within 20 minutes, treated with a mixture of 16.7 g of 3-methyl-3-butene-2-one and 32.4 g of dimethyl methoxymalonate at a temperature of 30-35° C. The mixture is stirred for 1 hour at a temperature of 35° C., and is then acidified with hydrochloric acid and extracted repeatedly with dichloromethane. The organic phases are washed with water, dried and concentrated. Crystallization from hot ethyl acetate and hexane gives pure methyl 2-hydroxy-1-methoxy-5-methyl-4-oxocyclohex-2-enecarboxylate of melting point 117-117.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06534445B1 |
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| 出典データセット | uspto-grants-2003_03 |
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| ORD ID | ord-24320ccc67c04b4f96aadf7909846525 |
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| 出典メモ | uspto-grants-2003_03 |
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