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Water → Dibenzo(b,f)thiepin-1-carboxylic acid, 10,11-dihydro-8-methoxy-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-Methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin | HCID 23337048 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Dibenzo(b,f)thiepin-1-carboxylic acid, 10,11-dihydro-8-methoxy- | HCID 3045903 | 69% |
反応手順
An amount of 6.0 g of potassium hydroxide was dissolved in 20 ml of 80% ethanol and to the solution was added 1 g of 2-methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin and the resulting mixture was refluxed for 26 hours. The mixture was freed of the solvent under reduced pressure to obtain the residue, which was dissolved in water and extracted with ethyl acetate. The aqueous layer was acidified with conc. hydrochloric acid and extracted with ethyl acetate. The extract was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate and freed of the solvent to give 743 mg (69%) of 2-methoxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin as pale reddish needles having a melting point of 185°-186° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04166127 |
| 出典データセット | uspto-grants-1979_08 |
| ORD ID | ord-e607eadbcebc4e6dbbd83bcd1976efa3 |
| 出典メモ | uspto-grants-1979_08 |