홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Ethyl Acetate → 2-(4-Isopropoxy-2-fluorophenyl)-1,2,4-triazine-3,5-dione

HRID 1488415
노트
인쇄 미리보기

반응식

HRID 1488415 반응식
[CH:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:16](=[O:17])[NH:15][C:14](=[O:18])[C:13](C(O)=O)=[N:12]2)=[C:7]([F:22])[CH:6]=1)([CH3:3])[CH3:2].C(=O)(O)[O-].[Na+].C(OCC)(=O)C>SCC(O)=O>[CH:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:16](=[O:17])[NH:15][C:14](=[O:18])[CH:13]=[N:12]2)=[C:7]([F:22])[CH:6]=1)([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 189810712-(4-Isopropoxy-2-fluorophenyl)-1,2,4-triazine-3,5-dion-6-carboxylic acid

생성물 1

HCID 189810222-(4-Isopropoxy-2-fluorophenyl)-1,2,4-triazine-3,5-dione수율 14.9%

시약·촉매·용매 1

HCID 1133Thioglycolic Acid용매

실험 절차

A solution of 4.70 g (0.0152 mole) of 2-(4-isopropoxy-2-fluorophenyl)-1,2,4-triazine-3,5-dion-6-carboxylic acid in 5 mL of mercaptoacetic acid was heated at 140°-145° C. for two hours under a nitrogen atmosphere. After this mixture had cooled, it was poured into 250 mL of a saturated aqueous solution of sodium bicarbonate with vigorous stirring. An equal volume of ethyl acetate was added to this mixture, and the resulting layers were separated. The organic layer was washed twice with 150 mL of a saturated aqueous solution of sodium bicarbonate and once with 150 mL of a saturated aqueous solution of sodium chloride. The organic solution was then dried over anhydrous magnesium sulfate and filtered. The solvent was evaporated under reduced pressure, leaving a syrup which slowly crystallized to a yellow-orange solid upon standing. This solid was recrystallized from ethyl acetate/petroleum ether (1:1), yielding 0.60 g of 2-(4-isopropoxy-2-fluorophenyl)-1,2,4-triazine-3,5-dione as a yellow solid. The NMR was consistent with the proposed structure. This reaction was repeated to obtain additional material for subsequent reactions.

후처리

  1. temperatureAfter this mixture had cooled
  2. customthe resulting layers were separated
  3. washThe organic layer was washed twice with 150 mL of a saturated aqueous solution of sodium bicarbonate and once with 150 mL of a saturated aqueous solution of sodium chloride
  4. dry with materialThe organic solution was then dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customThe solvent was evaporated under reduced pressure
  7. customleaving a syrup which
  8. customslowly crystallized to a yellow-orange solid
  9. customThis solid was recrystallized from ethyl acetate/petroleum ether (1:1)

출처 및 근거

ORD 기록
ord-27bc76a64fcd40759207d92bd9d07701
출처 데이터셋
uspto-grants-1997_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05674810

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트