Dimethylformamide → HCID 178477162, 화합물
반응식
[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]참가 물질
5
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-869c83d7a4f342b9a7564197938df829
- 출처 데이터셋
- uspto-grants-1994_10
- 특허 번호
- US05352792
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