Pyridine → HCID 22281167、化合物
反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH:7][S:8]([OH:11])(=[O:10])=[O:9].[C:12](OC(=O)C)(=[O:14])[CH3:13]>>[NH+:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:12]([O:9][S:8](=[O:11])(=[O:7])[O-:10])(=[O:14])[CH3:13]参加物
4
反応条件
- 温度
- 0 °C
実験手順
A mixture of 30 ml of acetic anhydride and 8.05 ml (0.1 mole) of pyridine is cooled to 0° C., and 5.4 ml of conc. H2SO4 is added dropwise at 0° C. under stirring. After 10 minutes, the crystals are filtered, washed with diethyl ether and dried under vacuum over P2O5 and KOH. Yield: 18.4 g (84%). IR: 1050 cm-1 sharp band, characteristic for sulfates and sulfate esters. Decomposes above 60° C., very hygroscopic. MW: 219.2 (C7H9O5NS).
後処理
- filtrationthe crystals are filtered
- washwashed with diethyl ether
- dry with materialdried under vacuum over P2O5 and KOH
- customDecomposes above 60° C.
出典と根拠
- ORDレコード
- ord-b87340ee322546868a52bdaab8ced4a8
- 出典データセット
- uspto-grants-1984_04
- 特許番号
- US04444682
反応ノート
読み込み中…