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

Water → 2-[(3-Bromophenyl)sulfonyl]-5-(4-chlorophenyl)-4-[(1E)-3,3,3-trifluoroprop-1-en-1-yl]-2,4-dihydro-3H-1,2,4-triazol-3-one

HRID 714669
노트
인쇄 미리보기

반응식

HRID 714669 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:9]([CH2:14][C@H:15](O)[C:16]([F:19])([F:18])[F:17])[C:10](=[O:13])[NH:11][N:12]=2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[Br:27][C:28]1[CH:29]=[C:30]([S:34](Cl)(=[O:36])=[O:35])[CH:31]=[CH:32][CH:33]=1.O>C(#N)C>[Br:27][C:28]1[CH:29]=[C:30]([S:34]([N:11]2[C:10](=[O:13])[N:9](/[CH:14]=[CH:15]/[C:16]([F:19])([F:18])[F:17])[C:8]([C:5]3[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=3)=[N:12]2)(=[O:36])=[O:35])[CH:31]=[CH:32][CH:33]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 17943m-Bromobenzenesulphonyl chlorideHCID 595368365-(4-Chlorophenyl)-4-[(2S)-3,3,3-trifluoro-2-hydroxypropyl]-2,4-dihydro-3H-1,2,4-triazol-3-one

생성물 1

HCID 699402022-[(3-Bromophenyl)sulfonyl]-5-(4-chlorophenyl)-4-[(1E)-3,3,3-trifluoroprop-1-en-1-yl]-2,4-dihydro-3H-1,2,4-triazol-3-one

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

500 mg (1.63 mmol) of the compound from Example 5A were dissolved in 10 ml of acetonitrile, and 449 mg (3.25 mmol) of potassium carbonate and 415 mg (1.63 mmol) of 3-bromobenzenesulfonyl chloride were added. The mixture was heated under reflux for 2 h. For work-up, 10 ml of water were added and the mixture was extracted twice with in each case 15 ml of ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and concentrated under reduced pressure. The crude product was purified by chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 8:1→5:1→1:1). This gave 285 mg (34% of theory) of the target compound.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 2 h
  3. extractionthe mixture was extracted twice with in each case 15 ml of ethyl acetate
  4. dry with materialThe combined organic phases were dried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe crude product was purified by chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate 8:1→5:1→1:1)

출처 및 근거

ORD 기록
ord-19ff9d4c50c8429e8836dc5a2becd0f2
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187466B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트