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Acetic Acid → 2-Benzylthio-5-methoxy-7-methyl[1,2,4]triazolo[1,5-a]pyridine

HRID 1940895
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HRID 1940895 반응식
[CH2:1]([S:8][C:9]1[N:19]=[C:12]2[CH:13]=[C:14]([CH3:18])[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.CCCCCC>CO.ClCCl>[CH2:1]([S:8][C:9]1[N:19]=[C:12]2[CH:13]=[C:14]([CH3:18])[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 8058HexaneHCID 10942334Sodium MethoxideHCID 190807642-Benzylthio-5-chloro-7-methyl[1,2,4]triazolo[1,5-a]pyridine

생성물 1

HCID 190807762-Benzylthio-5-methoxy-7-methyl[1,2,4]triazolo[1,5-a]pyridine

시약·촉매·용매 2

HCID 887Methanol용매2회
HCID 6344Dichloromethane용매

실험 절차

A mixture of 2-benzylthio-5-chloro-7-methyl[1,2,4]triazolo[1,5-a]pyridine (5.0 g, 0.017 mol), sodium methoxide in methanol (16 mL of 25 percent, 3.7 g, 0.070 mol) and methanol (100 mL) were heated at reflux with stirring for 4 hours. The reaction mixture was then cooled, acidified with acetic acid (10 mL), and concentrated by evaporation under reduced pressure. The residue obtained was dissolved in dichloromethane and the resulting solution was washed well with water, dried over magnesium sulfate, and concentrated by evaporation under reduced pressure. The residue obtained was mixed with hexane and filtered to recover the solids. The solids were dried to obtain 4.7 g (97 percent of theory) of the title compound as a tan powder melting an 85°-87° C.

후처리

  1. temperaturewere heated
  2. temperatureat reflux
  3. temperatureThe reaction mixture was then cooled
  4. concentrationconcentrated by evaporation under reduced pressure
  5. customThe residue obtained
  6. washthe resulting solution was washed well with water
  7. dry with materialdried over magnesium sulfate
  8. concentrationconcentrated by evaporation under reduced pressure
  9. customThe residue obtained
  10. filtrationfiltered
  11. customto recover the solids
  12. customThe solids were dried

출처 및 근거

ORD 기록
ord-efa51537fed74d4e81983426dbeecc43
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05700940

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