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

Methyl iodide → Methyl 4-fluoro-3-formylbenzoate

HRID 1966788
노트
인쇄 미리보기

반응식

HRID 1966788 반응식
[F:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[CH:11]=[O:12].CI.[C:15]([O-])([O-])=O.[K+].[K+]>CN(C=O)C.CCOC(C)=O.O>[CH3:15][O:7][C:6](=[O:8])[C:5]1[CH:9]=[CH:10][C:2]([F:1])=[C:3]([CH:11]=[O:12])[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 27948184-fluoro-3-formylbenzoic acid

생성물 1

HCID 53419692Methyl 4-fluoro-3-formylbenzoate수율 82%

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매
HCID 8857
Ethyl Acetate
용매

실험 절차

To a solution of 4-fluoro-3-formyl-benzoic acid (800 mg, 4.8 mmol) in DMF (10 mL), are added MeI (0.35 mL, 5.7 mmol) and K2CO3 (790 mg, 5.7 mmol). The reaction mixture is stirred at room temperature for 18 hours. The reaction mixture is diluted with EtOAc (20 mL) and water (10 mL). The organic layer is separated, washed with brine, dried under anhy. Na2SO4 (500 mg), filtered and is concentrated. The residue is purified by silica gel flash chromatography with 0-20% EtOAc/heptane as the eluent. The product fractions are collected and concentrated to afford 4-fluoro-3-formyl-benzoic acid methyl ester (710 mg, 82%).

후처리

  1. customThe organic layer is separated
  2. washwashed with brine
  3. customdried under anhy
  4. filtrationNa2SO4 (500 mg), filtered
  5. concentrationis concentrated
  6. customThe residue is purified by silica gel flash chromatography with 0-20% EtOAc/heptane as the eluent
  7. customThe product fractions are collected
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-61ad802bd44c407daddfad28287297f5
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420655B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트