Thiophosgene → 2,3-Dimethyl-4-nitrophenyl isothiocyanate
反応式
[CH3:1][C:2]1[C:8]([CH3:9])=[C:7]([N+:10]([O-:12])=[O:11])[CH:6]=[CH:5][C:3]=1[NH2:4].[C:13](Cl)(Cl)=[S:14]>C1(C)C=CC=CC=1>[CH3:1][C:2]1[C:8]([CH3:9])=[C:7]([N+:10]([O-:12])=[O:11])[CH:6]=[CH:5][C:3]=1[N:4]=[C:13]=[S:14]参加物
4
実験手順
To a solution of 2,3-dimethyl-4-nitroaniline (0.5 g, 1.0 equiv.) in toluene (50 mL) was added thiophosgene (0.3 mL, 1.3 equiv.) and the reaction mixture was heated at the reflux temp. overnight. The resulting mixture was concentrated under reduced pressure and the residue was purified by column chromatography (25% CH2Cl2/hex) to afford 2,3-dimethyl-4-nitrophenyl isothiocyanate as a light yellow solid (0.30 g, 48%): 1H NMR (CDCl3) δ2.39 (s, 3H), 2.41 (s, 3H), 7.20 (d, J=8.4 Hz, 1H); CI-MS m/z 200 ((M+H)+).
後処理
- temperaturethe reaction mixture was heated at the reflux temp
- customovernight
- concentrationThe resulting mixture was concentrated under reduced pressure
- customthe residue was purified by column chromatography (25% CH2Cl2/hex)
出典と根拠
- ORDレコード
- ord-d72828e659f34340a7d8282e5173f795
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06353006B1
反応ノート
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