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Potassium Hydroxide → 8-Chloro-2,4-dimethyl-5,6-dihydrobenzo[c]acridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 3,4-dihydro-5,7-dimethylnaphthalen-1(2H)-one | HCID 83619 | — |
| 反応物 | (2-Amino-6-chlorophenyl)methanol | HCID 21925574 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 8-Chloro-2,4-dimethyl-5,6-dihydrobenzo[c]acridine | HCID 71245114 | 67.4% |
反応手順
(2-Amino-6-chlorophenyl)methanol (16 g, 101 mmol), 5,7-dimethyl-3,4-dihydronaphthalen-1(2H)-one (20.0 g, 111 mmol), RuCl2(PPh3)3 (0.971 g, 1.01 mmol), and KOH (5.7 g, 101 mmol) were refluxed in 200 mL of toluene for 12 h. Water was collected from the reaction using a Dean-stark trap. The reaction mixture was allowed to cool to room temperature and filtered through a silica gel plug and eluted with dichloromethane. The product was washed by methanol and recrystallized from hexane to obtain ˜20 gram of the desired product which was confirmed by GC-MS.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09190621B2 |
| 出典データセット | uspto-grants-2015_11 |
| ORD ID | ord-87dd13e73e4f40b6a8134ba00e85ebdf |
| 出典メモ | uspto-grants-2015_11 |