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Water → 2-Benzyl-5-methoxy-2H-1,2,4,6-thiatriazin-3-one-1,1-dioxide

HRID 1982167
ノート
印刷プレビュー

反応式

HRID 1982167 の反応式
[C:1]([NH:5][C:6](=[N:9][S:10](=[O:20])(=[O:19])[NH:11][CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[O:7][CH3:8])(OC)=[O:2].[H-].[Na+].O>C1COCC1>[CH2:12]([N:11]1[C:1](=[O:2])[NH:5][C:6]([O:7][CH3:8])=[N:9][S:10]1(=[O:20])=[O:19])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 24758Sodium hydrideHCID 70392213N-carbomethoxy-N'-benzylsulfamoyl-O-methylisourea

生成物 1

HCID 136459252-Benzyl-5-methoxy-2H-1,2,4,6-thiatriazin-3-one-1,1-dioxide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of N-carbomethoxy-N'-benzylsulfamoyl-O-methylisourea (215 g) in anhydrous THF (200 ml) is added dropwise to a stirred suspension of sodium hydride (43 g of 60% dispersion) in anhydrous THF (900 ml) and refluxed for 2 hours under nitrogen. Water (800 ml) is added to the cooled reaction mixture and the aqueous mixture washed with ether. The pH of the aqueous layer is adjusted to about 3.2 and the resulting suspension extracted with methylene chloride. The methylene chloride extract is dried, filtered, and evaporated in vacuo. The residue is taken up in hot isopropyl alcohol, treated with charcoal, filtered hot, concentrated, cooled, the resulting precipitate filtered and dried in vacuo yielding the desired product, M.P.=141°-144° C.

後処理

  1. temperaturerefluxed for 2 hours under nitrogen
  2. washthe aqueous mixture washed with ether
  3. extractionthe resulting suspension extracted with methylene chloride
  4. extractionThe methylene chloride extract
  5. customis dried
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. additiontreated with charcoal
  9. filtrationfiltered hot
  10. concentrationconcentrated
  11. temperaturecooled
  12. filtrationthe resulting precipitate filtered
  13. customdried in vacuo

出典と根拠

ORDレコード
ord-bc33fff268a8452f81cf63882f15fb39
出典データセット
uspto-grants-1986_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04595683

反応ノート

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