Sodium Thiosulfate → UK-333747

HRID 2270925노트

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HRID 2270925 반응식
[Cl:1][C:2]1[C:3]([N:15]2[C:19]([C:20]3[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=3)=[N:18][N:17]=[C:16]2[CH2:26][O:27][CH3:28])=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[C:6](=[O:14])[NH:5]2.[OH:29]OS([O-])=O.[K+].S([O-])([O-])(=O)=S.[Na+].[Na+]>O>[Cl:1][C:2]1[C:3]([N:15]2[C:19]([C:20]3[CH:21]=[N+:22]([O-:29])[CH:23]=[CH:24][CH:25]=3)=[N:18][N:17]=[C:16]2[CH2:26][O:27][CH3:28])=[C:4]2[C:9](=[CH:10][C:11]=1[Cl:12])[NH:8][C:7](=[O:13])[C:6](=[O:14])[NH:5]2

참가 물질

5

반응물 3

HCID 24477Sodium ThiosulfateHCID 9802164HCID 9802164, 화합물HCID 23707502Potassium hydroxy sulfite

생성물 1

HCID 9867605UK-333747수율 85.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

(−)-6,7-Dichloro-5-[3-methoxymethyl-5-(3-pyridyl)-4H-1,2,4-triazol-4-yl]-2,3(1H,4H)-quinoxalinedione (see Preparation 1) (412.2 g, 0.98 mol) and OXONE (trade mark) (1.44 kg, 2.3 mol) were slurried in water (4.13 L) and the mixture stirred at ambient temperature for 60 hours. Saturated aqueous sodium thiosulphate solution (2.2 L) was added and the slurry stirred for 1 hour before being filtered under reduced pressure. The filter cake was slurried at ambient temperature for 4 hours in 1:1, by volume, isopropyl alcohol: dichloromethane (111 L) and the solid collected by filtration. The filtrate was vaporated under reduced pressure to give the title compound as a colourless solid (366 g).

후처리

  1. stirringthe slurry stirred for 1 hour
  2. filtrationbefore being filtered under reduced pressure
  3. waitThe filter cake was slurried at ambient temperature for 4 hours in 1:1, by volume, isopropyl alcohol
  4. filtrationdichloromethane (111 L) and the solid collected by filtration

출처 및 근거

ORD 기록
ord-d0ef3a47acb04335804b7fb10422c28d
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06333326B1

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