関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin | HCID 23337048 | — |
| 溶媒 | Diethylene Glycol | HCID 8117 | — |
| 生成物 | 2-Hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin | HCID 23337041 | 46% |
反応手順
An amount of 2.2 g of sodium hydroxide was dissolved in 30 ml of diethylene glycol by application of heat and to the mixture was added 2.2 g of 2-methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin and the resulting mixture was stirred at 200° C. for 16 hours. After cooling, to the mixture was added water and the mixture was extracted with ethyl acetate. The aqueous layer was acidified with conc. hydrochloric acid and extracted with ethyl acetate. This extract was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate and freed of the solvent to obtain the residue. This residue was recrystallized from benzene to afford 1.1 g (46%) of 2-hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin as brown crystals having a melting point of 210°-211° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04228284 |
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| 出典データセット | uspto-grants-1980_10 |
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| ORD ID | ord-603a21f55369406e860621300fd1d1fb |
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| 出典メモ | uspto-grants-1980_10 |
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