Water → N1,N3-dimethyl-N1-(thiazol-2-yl)propane-1,3-diamine
반응식
[CH3:1][NH:2][CH2:3][CH2:4][CH2:5][NH:6][CH3:7].Br[C:9]1[S:10][CH:11]=[CH:12][N:13]=1.O>C(Cl)(Cl)Cl>[CH3:1][N:2]([C:9]1[S:10][CH:11]=[CH:12][N:13]=1)[CH2:3][CH2:4][CH2:5][NH:6][CH3:7]참가 물질
5
반응 조건
- 온도
- 120 °C
실험 절차
2.45 g (24.0 mmol) N,N3-dimethylpropane-1,3-diamine was added to 0.36 ml (4.0 mmol) 2-bromothiazole and heated to 120° C. for 1 h. After cooling to RT, dilution with water and chloroform took place. The phases were separated and the aqueous phase was extracted with chloroform. The combined organic phases were dried over MgSO4, filtered, and concentrated in vacuo. Column chromatography (SiO2, DCE/MeOH/25% aq. NH3-soln 4:4:1) was carried out on the residue, yielding 440 mg (2.4 mmol, 59%) N1,N3-dimethyl-N1-(thiazol-2-yl)propane-1,3-diamine.
후처리
- temperatureAfter cooling to RT
- customThe phases were separated
- extractionthe aqueous phase was extracted with chloroform
- dry with materialThe combined organic phases were dried over MgSO4
- filtrationfiltered
- concentrationconcentrated in vacuo
출처 및 근거
- ORD 기록
- ord-a6ee07d53c424b61a6ce95f023a0907e
- 출처 데이터셋
- uspto-grants-2012_11
- 특허 번호
- US08318774B2
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