Sodium Thiosulfate → UK-333747

HRID 2270925ノート

反応式

HRID 2270925 の反応式
[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

参加物

5

反応物 3

HCID 24477Sodium ThiosulfateHCID 9802164HCID 9802164、化合物HCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 9867605UK-333747収率 85.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

(−)-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).

後処理

  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

出典と根拠

ORDレコード
ord-d0ef3a47acb04335804b7fb10422c28d
出典データセット
uspto-grants-2001_12
特許番号
US06333326B1

反応ノート

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