Hydrochloric Acid → Methyl 2-Fluoro-5-nitrobenzoate

HRID 80508

反応式

HRID 80508 の反応式
[F:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].Cl.[CH3:15]O>>[F:1][C:2]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][C:3]=1[C:4]([O:6][CH3:15])=[O:5]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 2809972-Fluoro-5-nitrobenzoic acid

生成物 1

HCID 11217860Methyl 2-Fluoro-5-nitrobenzoate

反応条件

温度
70 °C

実験手順

To a solution of 2-fluoro-5-nitrobenzoic acid (5 g, 27.0 mmol) in methanol (135 mL) was added HCl (2.66 mL, 32.4 mmol, 12.2M), and the mixture was heated with an oil bath at 70° C. for 24 hours. The solvent was evaporated, and the residue was dissolved in ethyl acetate and washed with saturated sodium bicarbonate and brine, dried over sodium sulfate, and concentrated to afford the title compound. 1H NMR (500 MHz, DMSO-d6) δ ppm 8.63 (dd, J=3.0, 6.2, 1H), 8.58-8.50 (m, 1H), 7.74-7.61 (m, 1H), 3.92 (s, 3H).

後処理

  1. customThe solvent was evaporated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with saturated sodium bicarbonate and brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-ea84a08026924be294c3a9119b20fc08
出典データセット
uspto-grants-2014_09
特許番号
US08846663B2

関連ノート

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