4,4'-Dimethoxybenzil → 5,6-bis-(4-methoxyphenyl)-1,2,4-triazin-3-thione

HRID 889829노트

반응식

HRID 889829 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([C:11]([C:13]2[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=2)=O)=O)=[CH:5][CH:4]=1.[NH2:21][NH:22][C:23]([NH2:25])=[S:24]>C(O)(=O)C.O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[C:11]([C:13]3[CH:18]=[CH:17][C:16]([O:19][CH3:20])=[CH:15][CH:14]=3)=[N:21][NH:22][C:23](=[S:24])[N:25]=2)=[CH:5][CH:4]=1

참가 물질

5

반응물 2

HCID 710434,4'-DimethoxybenzilHCID 2723789Thiosemicarbazide

생성물 1

HCID 42600365,6-bis-(4-methoxyphenyl)-1,2,4-triazin-3-thione수율 62.1%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

실험 절차

A mixture of 4,4′-dimethoxybenzil (13.6 g, 50 mmol) and 6.06 g of thiosemicarbazide (66.5 mmol) in 50 mL of glacial acetic acid were stirred at room temperature then refluxed overnight. The cooled reaction mixture was diluted with 150 mL of water and filtered. The solids were washed with water and dried. The crude product was heated with 55 mL of ethyl acetate, cooled, filtered and dried to give 10.1 g of 5,6-bis-(4-methoxyphenyl)-1,2,4-triazin-3-thione, mp 228–232° C.

후처리

  1. temperaturethen refluxed overnight
  2. customThe cooled reaction mixture
  3. filtrationfiltered
  4. washThe solids were washed with water
  5. customdried
  6. temperatureThe crude product was heated with 55 mL of ethyl acetate
  7. temperaturecooled
  8. filtrationfiltered
  9. customdried

출처 및 근거

ORD 기록
ord-9bb2a2711b9e4eb3bd3644ac0cfcf6b1
출처 데이터셋
uspto-grants-2006_02
특허 번호
US06995157B2

반응 노트

불러오는 중…