Ethylenediamine → N1-(4-Methyl-1,3-thiazol-2-YL)ethane-1,2-diamine
反応式
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]=1参加物
5
反応条件
- 温度
- 120 °C
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-29cfbb88ca444912943bb3ceb6246bb8
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09321724B2
反応ノート
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