Acetic Anhydride → HCID 9990006、化合物
反応式
[OH:1][CH2:2][C:3]([CH3:9])([CH3:8])[CH2:4][S:5][C:6]#[N:7].[C:10](OC(=O)C)(=[O:12])[CH3:11]>N1C=CC=CC=1>[C:10]([O:1][CH2:2][C:3]([CH3:9])([CH3:8])[CH2:4][S:5][C:6]#[N:7])(=[O:12])[CH3:11]参加物
4
実験手順
A mixture of 58.7 g of 3-hydroxy-2,2-dimethyl-1-propylthiocyanate, 400 ml of acetic anhydride and 400 ml of pyridine was stirred for 16 hours at room temperature. The reaction solution was concentrated under reduced pressure. The residue was dissolved in 500 ml of diethyl ether. The solution was washed in turn with 1N-hydrochloric acid, water, aqueous sodium hydrogen carbonate solution and water, and dried over anhydrous magnesium sulfate. After removing the solvent, the residue was purified by distillation under reduced pressure, thereby affording 53.2 g of 3-acetoxy-2,2-dimethyl-1-propylthiocyanate.
後処理
- concentrationThe reaction solution was concentrated under reduced pressure
- dissolutionThe residue was dissolved in 500 ml of diethyl ether
- washThe solution was washed in turn with 1N-hydrochloric acid, water, aqueous sodium hydrogen carbonate solution and water
- dry with materialdried over anhydrous magnesium sulfate
- customAfter removing the solvent
- distillationthe residue was purified by distillation under reduced pressure
出典と根拠
- ORDレコード
- ord-c00c62eaaf3346d88d3dde7544cda494
- 出典データセット
- uspto-grants-1992_10
- 特許番号
- US05155108
反応ノート
読み込み中…