Water → HCID 19806678、化合物
反応式
[Cl:1][C:2]1[C:3]([OH:8])=[N:4][S:5][C:6]=1[Cl:7].C(=O)([O-])[O-].[K+].[K+].[CH2:15](I)[CH3:16].O>CN(C=O)C>[Cl:1][C:2]1[C:3]([O:8][CH2:15][CH3:16])=[N:4][S:5][C:6]=1[Cl:7]参加物
6
実験手順
To a mixture of 4,5-dichloro-3-hydroxyisothiazole (17.00 g, 0.100 mol) and potassium carbonate (13.82 g, 0.100 mol) in dry DMF (80 ml) was added dropwise a solution of ethyl iodide (8.84 ml, 0.110 mol) in dry DMF (20 ml). The mixture was stirred 18 hours at ambient temperature. Water (500 ml) was added and the mixture was extracted with ether (3×400 ml). The combined ether extracts were dried over sodium sulfate, filtered, and concentrated in vacuo to give the crude product (18.35 g). The crude product was distilled to give 4,5-dichloro-3-ethoxyisothiazole (14.63 g, 74%, b.p. 64°-66°/0.1 mm). TLC (2% methanol/chloroform, silica): Rf=0.72.
後処理
- extractionthe mixture was extracted with ether (3×400 ml)
- dry with materialThe combined ether extracts were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give the crude product (18.35 g)
- distillationThe crude product was distilled
出典と根拠
- ORDレコード
- ord-67a87734d60e4d9b8b953ad89a1cfece
- 出典データセット
- uspto-grants-1992_12
- 特許番号
- US05171860
反応ノート
読み込み中…