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

HRID 1940910노트

반응식

HRID 1940910 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-96fb72c0a6a540d6afbb94bfd0fc6db5
출처 데이터셋
uspto-grants-1997_12
특허 번호
US05700940

반응 노트

불러오는 중…