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

HRID 42035

反応式

HRID 42035 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

HCID 2783401Methyl 2-amino-5-fluorobenzoate収率 42%

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-40ac5aa251c046e8afc1ac46c6d942ed
出典データセット
uspto-grants-2013_09
特許番号
US08536165B2

関連ノート

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