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Hydrochloric Acid → 2-Hydroxy-9-ethoxycarbonyl-10,11-dihydrodibenzo[b,f]thiepin
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | 2-Hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin | HCID 23337041 | — |
| 溶媒 | Benzene ethyl acetate | HCID 21583983 | — |
| 生成物 | 2-Hydroxy-9-ethoxycarbonyl-10,11-dihydrodibenzo[b,f]thiepin | HCID 12687125 | 85% |
反応手順
An amount of 1.7 g of 2-hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin was dissolved in 50ml of anhydrous ethanol and the mixture was refluxed for 3 hours, while hydrogen chloride gas was bubbled into the mixture. The solvent was distilled off to obtain the residue which was dissolved in the mixed solvent of ethyl acetate-benzene. The solution was washed with saturated sodium chloride solution and freed of solvent by distillation to obtain 1.6 g (85%) of 2-hydroxy-9-ethoxycarbonyl-10,11-dihydrodibenzo[b,f]thiepin as brown crystals having a melting point of 125°-129° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04228284 |
| 出典データセット | uspto-grants-1980_10 |
| ORD ID | ord-07fce35fe7bc4323945a6a1017ceb78e |
| 出典メモ | uspto-grants-1980_10 |