Dimethylformamide → HCID 178477162、化合物
反応式
[Na].[NH:2]1[CH:6]=[C:5]([SH:7])[N:4]=[N:3]1.[S:8]1[CH:12]=C[CH:10]=[C:9]1CC(OCCl)=O.CN(C)C=[O:22]>O>[C:9]([S:8][CH2:12][S:7][C:5]1[N:4]=[N:3][NH:2][CH:6]=1)(=[O:22])[CH3:10]参加物
5
実験手順
To a suspension of 1,2,3-triazole-4-thiol sodium salt (38 g: 309 mMol.) in dimethylformamide (150 ml) at -20° C. is added dropwise chloromethyl thiolacetate (37.4 g: 300 mMol.) over 10 minutes, and the mixture is stirred at the same temperature for 30 minutes and at room temperature for 2 hours, diluted with water and extracted with ethyl acetate. The extract is washed with water, aqueous sodium hydrogen carbonate, and water, dried over sodium sulfate, and concentrated under reduced pressure. The crystalline residue is washed with hexane, dried, and recrystallized from ether to give 4-acetylthiomethylthio-1,2,3-triazole (38.9 g). Yield: 69%. mp. 88° to 89° C.
後処理
- extractionextracted with ethyl acetate
- washThe extract is washed with water, aqueous sodium hydrogen carbonate, and water
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- washThe crystalline residue is washed with hexane
- customdried
- customrecrystallized from ether
出典と根拠
- ORDレコード
- ord-869c83d7a4f342b9a7564197938df829
- 出典データセット
- uspto-grants-1994_10
- 特許番号
- US05352792
反応ノート
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