Phosphorus oxychloride → HCID 68678410、化合物

HRID 2233017ノート

反応式

HRID 2233017 の反応式
[C:1]([N:5]1[C:18](=[O:19])[N:8]2[CH:9]=[C:10]([C:14]([CH3:17])([CH3:16])[CH3:15])[NH:11][C:12](=O)[C:7]2=[N:6]1)([CH3:4])([CH3:3])[CH3:2].P(Cl)(Cl)([Cl:22])=O>>[C:1]([N:5]1[C:18](=[O:19])[N:8]2[CH:9]=[C:10]([C:14]([CH3:17])([CH3:16])[CH3:15])[N:11]=[C:12]([Cl:22])[C:7]2=[N:6]1)([CH3:4])([CH3:3])[CH3:2]

参加物

3

反応物 2

HCID 24813Phosphorus oxychlorideHCID 68677556HCID 68677556、化合物

生成物 1

HCID 68678410HCID 68678410、化合物

実験手順

A solution of 5.90 g the product of Step D in phosphoryl chloride (100 mL) was heated to 110° C. After 16 h, the reaction mixture was cooled and the excess phosphoryl chloride was removed by distillation at reduced pressure (15 mm Hg). The residue was dissolved in chloroform and carefully poured onto 200 g of ice. After the ice had melted, the layers were separated and the aqueous was extracted with chloroform. The combined organic layers were washed with sat. sodium chloride solution, dried over sodium sulfate, filtered, and concentrated. The residue was purified by silica gel chromatography to yield 2-tert-butyl-8-chloro-6-tert-butyl-2H-[1,2,4]triazolo[4,3-a]pyrazin-3-one as a yellow solid. MS (M+H+)=283.3.

後処理

  1. temperaturethe reaction mixture was cooled
  2. customthe excess phosphoryl chloride was removed by distillation at reduced pressure (15 mm Hg)
  3. dissolutionThe residue was dissolved in chloroform
  4. additioncarefully poured onto 200 g of ice
  5. customthe layers were separated
  6. extractionthe aqueous was extracted with chloroform
  7. washThe combined organic layers were washed with sat. sodium chloride solution
  8. dry with materialdried over sodium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated
  11. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-f00ce380245e4616be43c32ed5237883
出典データセット
uspto-grants-2010_05
特許番号
US07709473B2

反応ノート

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