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2-Trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-on → 2-Trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-on | HCID 12687114 | — |
| 反応物 | HCID 178418435 | HCID 178418435 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-ol | HCID 12687116 | — |
反応手順
To the mixture of 2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-one obtained in Example 40 and 10 ml of methanol was gradually added 0.2 g of sodium boron hydride with ice-cooling over a period of 5 minutes and the mixture was reacted at room temperature for 30 minutes and refluxed for 15 minutes. After the completion of the reaction, methanol was distilled off. After cooling, to the mixture was added water and the mixture was extracted with chloroform. The extract was washed with water, dried over anhydrous sodium sulfate and freed of the solvent to obtain 0.5 g of 2-trifluoromethyl-9-chloro-10,11-dihydrodibenzo[b,f]thiepin-11-ol as colorless crystals having a melting point of 130°-132° 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-3325dc4f6ce54b34858198213e576066 |
| 出典メモ | uspto-grants-1979_08 |