Phosphorus oxychloride → 2H-1,2,4,6-Thiatriazine, 3-chloro-2,5-dimethyl-, 1,1-dioxide
反応式
[CH3:1][N:2]1[C:7](=O)[NH:6][C:5]([CH3:9])=[N:4][S:3]1(=[O:11])=[O:10].P(Cl)(Cl)(Cl)(Cl)[Cl:13].P(Cl)(Cl)(Cl)=O>>[Cl:13][C:7]1[N:2]([CH3:1])[S:3](=[O:11])(=[O:10])[N:4]=[C:5]([CH3:9])[N:6]=1参加物
4
反応条件
- 温度
- 110 °C
実験手順
212 parts of 2,5-dimethyl-2H-1,2,4,6-thiatriazin-3-one-1,1-dioxide were introduced into a stirred mixture of 292 parts of phosphorus pentachloride and 1,400 parts of phosphorus oxychloride at room temperature, and the mixture was heated to 110° C. in the course of 30 minutes. The reaction mixture was stirred under reflux for 6 hours and thereafter concentrated under reduced pressure, giving 234 parts (100% of theory) of 3-chloro-2,5-dimethyl-2H-1,2,4,6-thiatriazine-1,1-dioxide of: melting point 86°-90° C. (Compound No. 1) (NMR (60 MHz, CDCl3): CH3 -C 2.4δ, CH3 -N 3.68δ).
後処理
- temperatureunder reflux for 6 hours
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-5ccfd31efdab4921ae9a24f9efb1d0ac
- 出典データセット
- uspto-grants-1984_01
- 特許番号
- US04426219
反応ノート
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