Water → 3-Methyl-4-[((4-methyl-1-propylimidazol-5-yl)methyl)sulfanyl]aniline
반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([SH:8])=[C:4]([CH3:9])[CH:3]=1.C(N(CC)CC)C.Cl.Cl[CH2:19][C:20]1[N:24]([CH2:25][CH2:26][CH3:27])[CH:23]=[N:22][C:21]=1[CH3:28].O>O1CCCC1.CO>[CH3:9][C:4]1[CH:3]=[C:2]([CH:7]=[CH:6][C:5]=1[S:8][CH2:19][C:20]1[N:24]([CH2:25][CH2:26][CH3:27])[CH:23]=[N:22][C:21]=1[CH3:28])[NH2:1]참가 물질
반응물 4
생성물 1
시약·촉매·용매 2
실험 절차
To a solution of 4-amino-2-methylthiophenol (500 mg) and triethylamine (3.0 ml) in tetrahydrofuran (15 ml) was added dropwise a solution of 5-chloromethyl-4-methyl-1-propylimidazole hydrochloride (908 mg) in methanol (5 ml) at 0° C. under argon atmosphere, after which the mixture was returned to room temperature and stirred for 3 hours. Water was added and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine and dried with magnesium sulfate. The solvent was distilled off under reduced pressure, and the resulting residue was purified by basic silica gel column chromatography (hexane:ethyl acetate=1:1→ethyl acetate) to give 3-methyl-4-[((4-methyl-1-propylimidazol-5-yl)methyl)sulfanyl]aniline (301 mg) as a brown powder.
후처리
- customwas returned to room temperature
- extractionthe mixture was extracted with ethyl acetate
- washThe organic layer was washed with saturated brine
- dry with materialdried with magnesium sulfate
- distillationThe solvent was distilled off under reduced pressure
- customthe resulting residue was purified by basic silica gel column chromatography (hexane:ethyl acetate=1:1→ethyl acetate)
출처 및 근거
- ORD 기록
- ord-f1bc5ef4b8d04464a7d13fa7b7d44da2
- 출처 데이터셋
- uspto-grants-2013_01
- 특허 번호
- US08362058B2
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