3,4-Dichloro-2-methyl-5-ethoxycarbonylisothiazolium fluorosulfonate → 4-Chloro-5-ethoxycarbonyl-2-methyl-4-isothiazolin-3-one
反応式
FS([O-])(=O)=[O:3].Cl[C:7]1[C:11]([Cl:12])=[C:10]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[S:9][N+:8]=1[CH3:18]>C([O-])([O-])=O.[K+].[K+]>[Cl:12][C:11]1[C:7](=[O:3])[N:8]([CH3:18])[S:9][C:10]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14]参加物
3
実験手順
3,4-Dichloro-5-ethoxycarbonyl-2-methylisothiazolium fluorosulfonate (4.2 g, 0.012 mol) was added to 50 ml of saturated K2CO3 solution. The aqueous phase was extracted with 3×50 ml of CH2Cl2. Then combined extracts were dried (MgSO4), filtered and conc. to yield a solid. Recrystallization from heptane yielded 1.0 g (35%) of 4-chloro-5-ethoxycarbonyl-2-methyl-4-isothiazolin-3-one, mp 142-147.
後処理
- extractionThe aqueous phase was extracted with 3×50 ml of CH2Cl2
- dry with materialThen combined extracts were dried (MgSO4)
- filtrationfiltered
- customconc. to yield a solid
- customRecrystallization from heptane
出典と根拠
- ORDレコード
- ord-21f276798cbe472f9feee595215a9664
- 出典データセット
- uspto-grants-1981_07
- 特許番号
- US04281136
反応ノート
読み込み中…