Benzenamine, 3,5-bis(trifluoromethyl)- → Phenyl [3,5-bis(trifluoromethyl)phenyl]carbamate
反応式
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:4]=[C:5]([CH:7]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:9]=1)[NH2:6].C(N(CC)C(C)C)(C)C.Cl[C:26]([O:28][C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)=[O:27]>ClCCl>[C:29]1([O:28][C:26](=[O:27])[NH:6][C:5]2[CH:4]=[C:3]([C:2]([F:14])([F:15])[F:1])[CH:9]=[C:8]([C:10]([F:11])([F:12])[F:13])[CH:7]=2)[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1参加物
実験手順
3,5-Bis-(trifluoromethyl)aniline (2.0 g, 8.7 mmol) was dissolved in dichloromethane (80 mL) and N,N-diisopropylethylamine (1.6 mL, 9.6 mmol) was added followed by slow addition of phenyl chloroformate (1.1 mL, 8.7 mmol). The resulting mixture was stirred at room temperature for 16 hours. The mixture was successively washed with 1N hydrochloric acid (3×100 mL), water (3×100 mL), a mixture of water and saturated aqueous sodium hydrogen carbonate (1:1, 2×100 mL) and a mixture of water and saturated aqueous sodium chloride (1:1, 3×100 mL), dried (MgSO4) and concentrated in vacuo. The residue was crystallised from heptane containing a little diethyl ether to afford 1.3 g (43%) of (3,5-bis-trifluoromethylphenyl)carbamic acid phenyl ester as a solid.
後処理
- washThe mixture was successively washed with 1N hydrochloric acid (3×100 mL), water (3×100 mL)
- additiona mixture of water and saturated aqueous sodium hydrogen carbonate (1:1, 2×100 mL)
- additiona mixture of water and saturated aqueous sodium chloride (1:1, 3×100 mL)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo
- customThe residue was crystallised from heptane containing a little diethyl ether
出典と根拠
- ORDレコード
- ord-66ae1d6ffe444e1d9824c37a2af30a7a
- 出典データセット
- uspto-grants-2003_01
- 特許番号
- US06503949B1
反応ノート
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