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Methanol → 10,11-Dihydrodibenzo(b,f)(1,4)thiazepine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Dibenzothiazepinone | HCID 374829 | — |
| 反応物 | (Dimethyl sulfide)trihydroboron | HCID 12423031 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 10,11-Dihydrodibenzo(b,f)(1,4)thiazepine | HCID 12310482 | — |
反応手順
To a mixture of 3.3 g of 10,11-dihydro-11-oxodibenz[b,f][1,4]thiazepine in 25 ml of tetrahydrofuran is added 4.0 ml of 10 molar borane-dimethylsulfide in tetrahydrofuran. The mixture is stirred at room temperature for 18 hours, 50 ml of anhydrous methanol added and the solvent removed. An additional 30 ml of methanol is added and the solvent removed to give white crystals. A sample is purified by chromatography on silica gel with hexane-chloroform-ethyl acetate (2:1:1) as solvent to give white crystals, m.p. 145°-148° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05834461 |
| 出典データセット | uspto-grants-1998_11 |
| ORD ID | ord-39c2414928ca4ba296ae3349d9d22d6f |
| 出典メモ | uspto-grants-1998_11 |