3-Methoxyaniline → (3-Methoxy-phenylamino)-phenyl-acetic acid

HRID 76998

반응식

HRID 76998 반응식
Br[CH:2]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[C:3]([OH:5])=[O:4].[CH3:12][O:13][C:14]1[CH:15]=[C:16]([CH:18]=[CH:19][CH:20]=1)[NH2:17]>C1COCC1>[CH3:12][O:13][C:14]1[CH:15]=[C:16]([NH:17][CH:2]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:3]([OH:5])=[O:4])[CH:18]=[CH:19][CH:20]=1

참가 물질

4

반응물 2

HCID 108243-MethoxyanilineHCID 97919Bromo(phenyl)acetic acid

생성물 1

HCID 2759625(3-Methoxy-phenylamino)-phenyl-acetic acid수율 99%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 2-bromo-2-phenylacetic acid (0.5 g, 2.28 mmol) and 3-methoxyaniline (0.54 mL, 4.56 mmol) in THF (12 mL) is refluxed for 4 hours. Solvent is removed under vacuum, the residue is taken up with 1M HCl and extracted with EtOAc. The organic phase is dried (Na2SO4), filtered and evaporated. The crude is purified by flash chromatography (DCM/MeOH=98/2 to 9/1) to obtain intermeaditae I116 as a white solid (0.58 g, 99% yield).

후처리

  1. customSolvent is removed under vacuum
  2. extractionextracted with EtOAc
  3. dry with materialThe organic phase is dried (Na2SO4)
  4. filtrationfiltered
  5. customevaporated
  6. customThe crude is purified by flash chromatography (DCM/MeOH=98/2 to 9/1)

출처 및 근거

ORD 기록
ord-d2075340269f4f199e1ba8a3ca303395
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08835682B2

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