Methylamine → 1-(3,4-dichlorophenyl)-3-methylthiourea
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]=[C:9]=[S:10])=[CH:4][C:3]=1[Cl:11].[CH3:12][NH2:13]>C(O)C>[Cl:11][C:3]1[CH:4]=[C:5]([NH:8][C:9]([NH:13][CH3:12])=[S:10])[CH:6]=[CH:7][C:2]=1[Cl:1]参加物
4
反応条件
- 温度
- 80 °C
実験手順
To a stirred solution of 1,2-dichloro-4-isothiocyanatobenzene (1 g, 4.9 mmol) in ethanol (30 mL) was added 8M methyl amine in ethanol (0.613 mL, 4.9 mmol) and the reaction was heated at 80° C. overnight. The solvent was removed under vacuum and the residue was washed with diethyl ether (10 mL) and dried to give crude 1-(3,4-dichlorophenyl)-3-methylthiourea as an off white solid (0.8 g, 69%). 1HNMR: 400 MHz, DMSO-d6: δ 2.93 (d, J=4.40 Hz, 3H), 7.37 (d, J=7.60 Hz, 1H), 7.55 (d, J=8.40 Hz, 1H), 7.86 (d, J=2.40 Hz, 1H), 7.92 (bs, 1H), 9.74 (bs, 1H).
後処理
- customThe solvent was removed under vacuum
- washthe residue was washed with diethyl ether (10 mL)
- customdried
出典と根拠
- ORDレコード
- ord-ba1422761c6f4212891d4e08d313ca5d
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08722670B2
反応ノート
読み込み中…