4-Bromo-2-nitro-cyclopropylbenzene → Tranylcypromine
反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:10][CH:9]2[N+:11]([O-])=O)=[CH:4][CH:3]=1>C(O)C.[Pd]>[NH2:11][CH:9]1[CH2:10][CH:8]1[C:5]1[CH:6]=[CH:7][CH:2]=[CH:3][CH:4]=1参加物
4
実験手順
3.5 g of 4-bromo-2-nitro-cyclopropylbenzene are dissolved in 30 ml of ethanol and, after addition of 0.5 g of palladium-on-charcoal (10%), are hydrogenated in a Parr apparatus at room temperature under a hydrogen pressure of 5 bar for 2.5 hours. After cooling, the solvent is distilled off in a rotary evaporator and the residue is rendered alkaline with 1N sodium hydroxide solution and extracted three times with 50 ml of ether each time. The combined organic phases are dried over sodium sulphate, the solvent is distilled off in a rotary evaporator and the residue is purified by column chromatography.
後処理
- customare hydrogenated in a Parr apparatus at room temperature under a hydrogen
- customfor 2.5 hours
- temperatureAfter cooling
- distillationthe solvent is distilled off in a rotary evaporator
- extractionextracted three times with 50 ml of ether each time
- dry with materialThe combined organic phases are dried over sodium sulphate
- distillationthe solvent is distilled off in a rotary evaporator
- customthe residue is purified by column chromatography
出典と根拠
- ORDレコード
- ord-d9f7ea18dee34b04aa88c425d1b95bf5
- 出典データセット
- uspto-grants-1998_01
- 特許番号
- US05707989
反応ノート
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