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Piperazine → 1-(10,11-Dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)piperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | 5H-Dibenzo(a,d)cycloheptene, 10,11-dihydro-5-chloro- | HCID 14587 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-(10,11-Dihydro-5H-dibenzo[a,d]cyclohepten-5-yl)piperazine | HCID 2735936 | 2,915.9% |
反応手順
Into a solution of partially dissolved piperazine (15.2 g, 0.17 mmol) in THF (130 mL) at more temperature was added dropwise a solution of 5-chloro-10,11-dihydro-5H-dibenzo[a,d]cycloheptene (2.3g, 10.3 mmol) in 20 mL THF. The reaction was allowed to stir overnight and then was diluted with CH2Cl2, washed once with 1.0N NaOH solution, once with brine and then dried (Mg SO4). It was then filtered and the solvent removed to give a residue which was flash chromatographed (5% MeOH saturated with NH3 in CH2Cl2) to give 1.38 g of a glassy solid of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05416087 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-70f3f48392af48ca9feb3ad8a30df0a3 |
| 出典メモ | uspto-grants-1995_05 |