Hydrochloric Acid → 2-Methyl-4-aminobiphenyl hydrochloride
反応式
O.[ClH:2].[CH3:3][C:4]1[CH:9]=[C:8]([NH:10]C(C)=O)[CH:7]=[CH:6][C:5]=1[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(O)(=O)C>[ClH:2].[CH3:3][C:4]1[CH:9]=[C:8]([NH2:10])[CH:7]=[CH:6][C:5]=1[C:14]1[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1参加物
5
実験手順
300 g of water and 296 g of HCl (37%) are added to the 2-methyl-4-acetaminobiphenyl prepared as described in Example 1. Any chlorobenzene still present is distilled off azeotropically, and the mixture is subsequently refluxed until HPLC monitoring indicates complete conversion (about 4 hours). The suspension obtained can be reacted further without further purification and without removal of the acetic acid formed as coproduct in the cleavage. The yield is (calculated from HPLC percentages by area) 99%.
後処理
- customprepared
- distillationAny chlorobenzene still present is distilled off azeotropically
- temperaturethe mixture is subsequently refluxed until HPLC monitoring
- customconversion (about 4 hours)
- customThe suspension obtained can
- customformed as coproduct in the cleavage
出典と根拠
- ORDレコード
- ord-8a894b2f7d324691a6aeecead6b50a5b
- 出典データセット
- uspto-grants-2003_05
- 特許番号
- US06566546B2
反応ノート
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