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Diisobutylaluminumhydride → 10,11-Dihydro-2,8-dimethyl-5H-dibenzo[a,d]cyclohepten-5-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisobutylaluminumhydride | HCID 21225700 | — |
| 反応物 | 10,11-dihydro-2,8-dimethyl-5H-dibenzo[a,d]cyclohepten-5-one | HCID 22117201 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 10,11-Dihydro-2,8-dimethyl-5H-dibenzo[a,d]cyclohepten-5-ol | HCID 18689747 | — |
反応手順
Diisobutylaluminium hydride (5.5 ml of a 1M solution in tetrahydrofuran) was added dropwise to 10,11-dihydro-2,8-dimethyl-5H-dibenzo[a,d]cyclohepten-5-one (European Patent, 1993, 0 589 322 A1) (1.2 g) in tetrahydrofuran (20 ml) at-78 ° C. After 1 hour the cooling bath was removed and the reaction was stirred at r.t. for 2 hours. The reaction was quenched with brine and methanol. After 0.5 hours the reaction was partitioned between ethyl acetate and water. The ethyl acetate solution was washed with water, brine, dried (MgSO4) and evaporated. Purification was by chromatography eluting with toluene. Yield 1.2 g. Used directly in step (ii)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06107297 |
| 出典データセット | uspto-grants-2000_08 |
| ORD ID | ord-e02be76acde146da86d947344c9547d5 |
| 出典メモ | uspto-grants-2000_08 |