Ethylenediamine → N1-(4-Methyl-1,3-thiazol-2-YL)ethane-1,2-diamine
반응식
Br[C:2]1[S:3][CH:4]=[C:5]([CH3:7])[N:6]=1.[CH2:8]([NH2:11])[CH2:9][NH2:10].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH3:7][C:5]1[N:6]=[C:2]([NH:10][CH2:9][CH2:8][NH2:11])[S:3][CH:4]=1참가 물질
5
반응 조건
- 온도
- 120 °C
실험 절차
A mixture of 2-bromo-4-methylthiazole (502 mg, 2.82 mmol), ethylenediamine (15 mL, 224 mmol) and potassium carbonate (780 mg, 5.64 mmol) was heated under microwave heating at 120° C. for 30 min in a closed vial. Ethanol (200 mL) was added, the resulting mixture was filtered, the solids washed with EtOH and the combined filtrates concentrated under reduced pressure. The residue was mixed with toluene and concentrated under reduced pressure; this step was repeated two times after which 620 mg of a solid was obtained that was used directly in the next step.
후처리
- temperaturewas heated under microwave
- filtrationthe resulting mixture was filtered
- washthe solids washed with EtOH
- concentrationthe combined filtrates concentrated under reduced pressure
- additionThe residue was mixed with toluene
- concentrationconcentrated under reduced pressure
- customwas obtained
출처 및 근거
- ORD 기록
- ord-29cfbb88ca444912943bb3ceb6246bb8
- 출처 데이터셋
- uspto-grants-2016_04
- 특허 번호
- US09321724B2
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