Potassium Fluoride → HCID 178456692、化合物
反応式
[CH:1]([N:4]1[C:8](Cl)=[N:7][C:6]([OH:10])=[N:5]1)([CH3:3])[CH3:2].[F-:11].[K+]>S1(CCCC1)(=O)=O>[CH:1]([N:4]1[C:8]([F:11])=[N:7][C:6]([OH:10])=[N:5]1)([CH3:3])[CH3:2]参加物
4
実験手順
16.2 g of 1-isopropyl-5-chloro-3-hydroxy-1,2,4-triazole, 29 g of dry potassium fluoride and 150 ml of sulpholane are heated together for 16 hours to 160°-200°C. The solvent is evaporated in a high vacuum and the residue then treated with 10 % acetic acid and extracted with ethyl acetate. The ethyl acetate is evaporated off and the residueal solid is recrystallised from water, in the process of which 1-isopropyl-5-fluoro-3-hydroxy-1,2,4-triazole is obtained in the form of white crystals with a melting point of 80°-95°C. The product can be recrystallised from an organic solvent in order to purify it further.
後処理
- customThe solvent is evaporated in a high vacuum
- additionthe residue then treated with 10 % acetic acid
- extractionextracted with ethyl acetate
- customThe ethyl acetate is evaporated off
- customthe residueal solid is recrystallised from water, in the process of which 1-isopropyl-5-fluoro-3-hydroxy-1,2,4-triazole
- customis obtained in the form of white crystals with a melting point of 80°-95°C
- customThe product can be recrystallised from an organic solvent in order
- customto purify it further
出典と根拠
- ORDレコード
- ord-cd673947d4b740c198cdf22a8fe14316
- 出典データセット
- uspto-grants-1976_01
- 特許番号
- US03932629
反応ノート
読み込み中…