Hydrochloric Acid → Methyl 2-Fluoro-5-nitrobenzoate

HRID 80508

반응식

HRID 80508 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

HCID 11217860Methyl 2-Fluoro-5-nitrobenzoate

반응 조건

온도
70 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ea84a08026924be294c3a9119b20fc08
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846663B2

연결된 노트

불러오는 중…