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

HRID 2295696노트

반응식

HRID 2295696 반응식
P(Cl)(Cl)(Cl)(Cl)Cl.[CH3:7][N:8]1[C:13](=O)[NH:12][C:11]([CH2:15][CH3:16])=[N:10][S:9]1(=[O:18])=[O:17].P(Cl)(Cl)([Cl:21])=O>ClCCCl>[Cl:21][C:13]1[N:8]([CH3:7])[S:9](=[O:18])(=[O:17])[N:10]=[C:11]([CH2:15][CH3:16])[N:12]=1

참가 물질

5

반응물 3

HCID 24813Phosphorus oxychlorideHCID 24819Phosphorus pentachlorideHCID 1588642H-1,2,4,6-Thiatriazin-3(4H)-one, 5-ethyl-2-methyl-, 1,1-dioxide

생성물 1

HCID 1588672H-1,2,4,6-Thiatriazine, 3-chloro-5-ethyl-2-methyl-, 1,1-dioxide

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

110 parts of phosphorus pentachloride were added to a stirred mixture of 86 parts of 2-methyl-5-ethyl-2H-1,2,4,6-thiatriazine-3-one-1,1-dioxide, 100 parts of 1,2-dichloroethane and 112 parts of phosphorus oxychloride at room temperature. The reaction mixture was then stirred under reflux for 12 hours. After concentration, 94 parts (100% of theory) of 3-chloro-2-methyl-5-ethyl-2H-1,2,4,6-thiatriazine-1,1-dioxide of nD25 =1.5331 were obtained. (NMR (60 MHz, CDCl3): CH3 -N 3.7δ). The very pure product (nD25 =1.5337) boils at 123°-125° C./0.2 mbar (Compound No. 3).

후처리

  1. temperatureunder reflux for 12 hours
  2. concentrationAfter concentration, 94 parts (100% of theory) of 3-chloro-2-methyl-5-ethyl-2H-1,2,4,6-thiatriazine-1,1-dioxide of nD25 =1.5331
  3. customwere obtained

출처 및 근거

ORD 기록
ord-7694bc65687747c399efa2e3277182bc
출처 데이터셋
uspto-grants-1984_01
특허 번호
US04426219

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