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

1-Bromo-2-methylpropane → 6-(3-fluoro-4-methylphenyl)-2-isobutyl-4-methoxycarbonyl-2H-pyridazin-3-one

HRID 7911
노트
인쇄 미리보기

반응식

HRID 7911 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:10]=[C:11]([C:16]([O:18][CH3:19])=[O:17])[C:12](=[O:15])[NH:13][N:14]=2)[CH:5]=[CH:6][C:7]=1[CH3:8].C(=O)([O-])[O-].[K+].[K+].[CH2:26](Br)[CH:27]([CH3:29])[CH3:28].C(=O)([O-])O.[Na+]>CN(C)C=O>[F:1][C:2]1[CH:3]=[C:4]([C:9]2[CH:10]=[C:11]([C:16]([O:18][CH3:19])=[O:17])[C:12](=[O:15])[N:13]([CH2:26][CH:27]([CH3:29])[CH3:28])[N:14]=2)[CH:5]=[CH:6][C:7]=1[CH3:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 65551-Bromo-2-methylpropaneHCID 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 219914756-(3-fluoro-4-methylphenyl)-4-methoxycarbonyl-2H-pyridazin-3-one

생성물 1

HCID 219914926-(3-fluoro-4-methylphenyl)-2-isobutyl-4-methoxycarbonyl-2H-pyridazin-3-one수율 85%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

반응 조건

온도
80 °C

실험 절차

To a solution of 6-(3-fluoro-4-methylphenyl)-4-methoxycarbonyl-2H-pyridazin-3-one (5.28 g, 20.0 mmol) in N,N-dimethylformamide (40 mL) were added potassium carbonate (5.53 g, 40.0 mmol) and isobutyl bromide (3.29 g, 24.0 mmol), and the mixture was stirred at 80° C. for 1 hour. The temperature of the reaction mixture was allowed to drop back to room temperature. A saturated aqueous solution of sodium hydrogencarbonate was added, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure. The residue was purified by column chromatography on silica gel [silica gel 100 g, chloroform/methanol (100/1→50/1)) to yield the title compound as an orange oil (5.41 g, 84.9%).

후처리

  1. customto drop back to room temperature
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe extract was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel [silica gel 100 g, chloroform/methanol (100/1→50/1))

출처 및 근거

ORD 기록
ord-447057a76e4c472e8ee185e270a27f68
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07087606B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트