Acetic Acid → 2-Benzylthio-8-chloro-5-methoxy[1,2,4]triazolo[1,5-a]pyridine

HRID 1898818ノート

反応式

HRID 1898818 の反応式
[CH2:1]([S:8][C:9]1[N:19]=[C:12]2[C:13]([Cl:18])=[CH:14][CH:15]=[C:16](Cl)[N:11]2[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[O-].[Na+].[C:23](O)(=[O:25])C>CO>[CH2:1]([S:8][C:9]1[N:19]=[C:12]2[C:13]([Cl:18])=[CH:14][CH:15]=[C:16]([O:25][CH3:23])[N:11]2[N:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 10942334Sodium MethoxideHCID 190807452-Benzylthio-5,8-dichloro[1,2,4]triazolo[1,5-a]pyridine

生成物 1

HCID 190807292-Benzylthio-8-chloro-5-methoxy[1,2,4]triazolo[1,5-a]pyridine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

2-Benzylthio-5,8-dichloro[1,2,4]triazolo[1,5-a]pyridine (6.0 g, 0.019 mol) and 25 percent sodium methoxide in methanol (26.5 mL, 6.3 g, 0.116 mol) were combined in methanol and the mixture was heated to reflux for 2 hours. The mixture was then cooled, acidified with acetic acid, and concentrated by evaporation under reduced pressure. The residue was dissolved in dichloromethane and the solution was washed with water and concentrated by evaporation under reduced pressure. The residue was triturated with hexane and the resulting solids were collected by filtration and dried to obtain 5.76 g 99 percent of theory) of the title compound as a light tan powder melting at 90°-91° C.

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 2 hours
  3. temperatureThe mixture was then cooled
  4. concentrationconcentrated by evaporation under reduced pressure
  5. dissolutionThe residue was dissolved in dichloromethane
  6. washthe solution was washed with water
  7. concentrationconcentrated by evaporation under reduced pressure
  8. customThe residue was triturated with hexane
  9. filtrationthe resulting solids were collected by filtration
  10. customdried

出典と根拠

ORDレコード
ord-961fa4efb2af4563b4b58fbea26ef33c
出典データセット
uspto-grants-1996_11
特許番号
US05571775

反応ノート

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