4-Chlorotoluene → N,N-diethyl-p-toluidine
反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1.[CH2:9]([NH:11][CH2:12][CH3:13])[CH3:10].CC([O-])(C)C.[K+]>C1(C)C=CC=CC=1>[CH2:9]([N:11]([C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][CH:3]=1)[CH2:12][CH3:13])[CH3:10]参加物
5
実験手順
20 mmol of p-chlorotoluene (2.53 g), 24 mmol of diethylamine (1.75 g), 28 mmol of KOtBu (3.13 g) and 44 mg of trans-di-μ-acetatobis[2-[bis(1,1-dimethylethyl)-phosphino]-2-methylpropyl-C,P]dipalladium(II) (0.3 mol %) are suspended in 50 ml of toluene and refluxed for 24 hours. After cooling to room temperature, the salts are filtered off and washed with petroleum ether. The solvents are removed from the filtrate on a rotary evaporator. Distillation via a bulb tube (100° C./12 torr) gives 4-(N,N-diethylamino)toluene as a colorless liquid in a yield of 87%.
後処理
- temperaturerefluxed for 24 hours
- filtrationthe salts are filtered off
- washwashed with petroleum ether
- customThe solvents are removed from the filtrate on a rotary evaporator
- distillationDistillation via a bulb tube (100° C./12 torr)
出典と根拠
- ORDレコード
- ord-933c0acdf73e4d5ab48e48b6f7640958
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06353136B1
反応ノート
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