2-Amino-5-fluorobenzoic acid → Methyl 2-amino-5-fluorobenzoate

HRID 42035

반응식

HRID 42035 반응식
[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Cl.[CH3:13]O>>[NH2:1][C:2]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:3]=1[C:4]([O:6][CH3:13])=[O:5]

참가 물질

3

반응물 2

HCID 1014122-Amino-5-fluorobenzoic acidHCID 21893726Hydrochloride methanol

생성물 1

HCID 2783401Methyl 2-amino-5-fluorobenzoate수율 42%

반응 조건

온도
100 °C

실험 절차

A solution of 2-amino-5-fluorobenzoic acid (9.29 mmol, 1.440 g) in a mixture of HCl/MeOH (3N, 30 ml) was heated at 100° C. overnight. The solvent was evaporated and the crude mixture was extracted between DCM and K2CO3 saturated aqueous solution. The organic phase was evaporated and the crude mixture was purified by chromatography over SiO2 with hexane/ethyl acetate mixtures affording 0.650 g (yield 42%) of the expected product.

후처리

  1. customThe solvent was evaporated
  2. extractionthe crude mixture was extracted between DCM and K2CO3 saturated aqueous solution
  3. customThe organic phase was evaporated
  4. customthe crude mixture was purified by chromatography over SiO2 with hexane/ethyl acetate

출처 및 근거

ORD 기록
ord-40ac5aa251c046e8afc1ac46c6d942ed
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536165B2

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