Methylamine → 1-(3,4-dichlorophenyl)-3-methylthiourea
반응식
[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]참가 물질
4
반응 조건
- 온도
- 80 °C
실험 절차
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).
후처리
- customThe solvent was removed under vacuum
- washthe residue was washed with diethyl ether (10 mL)
- customdried
출처 및 근거
- ORD 기록
- ord-ba1422761c6f4212891d4e08d313ca5d
- 출처 데이터셋
- uspto-grants-2014_05
- 특허 번호
- US08722670B2
반응 노트
불러오는 중…