Phosphorus oxychloride → 2H-1,2,4,6-Thiatriazine, 3-chloro-2,5-dimethyl-, 1,1-dioxide

反応式

[CH3:1][C:2]1[NH:3][S:4](=[O:11])(=[O:10])[N:5]([CH3:9])[C:6](=O)[N:7]=1.P(Cl)(Cl)(Cl)(Cl)[Cl:13].P(Cl)(Cl)(Cl)=O>>[Cl:13][C:6]1[N:5]([CH3:9])[S:4](=[O:11])(=[O:10])[N:3]=[C:2]([CH3:1])[N:7]=1

参加物

反応物 3

HCID 24813Phosphorus oxychloride

HCID 24819Phosphorus pentachloride

HCID 178433508HCID 178433508、化合物

生成物 1

HCID 1588652H-1,2,4,6-Thiatriazine, 3-chloro-2,5-dimethyl-, 1,1-dioxide収率 100%

反応条件

温度: 110 °C

実験手順

212 parts of 3,6-dimethyl-6H-1,2,4,6-thiatriazin-5-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 then evaporated down under reduced pressure to give 234 parts (yield: 100% of theory) of 5-chloro-3,6-dimethyl-6H-1,2,4,6-thiatriazine-1,1-dioxide of melting point 86°-90° C. NMR (60 MHz, CDCl3): CH3 --C 2.4δ, CH3 --N 3.68).

後処理

temperatureunder reflux for 6 hours
customevaporated down under reduced pressure

出典と根拠

ORDレコード: ord-a4a038a0b0d3494b922539df1df58ad3
出典データセット: uspto-grants-1984_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US04472191

反応ノート

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