Hydrochloric Acid → 4-(5-Fluoro-2-(methyloxy)-4-pyridinyl)-3-((methyloxy)carbonyl)benzoic acid

HRID 1662537노트

반응식

HRID 1662537 반응식
[F:1][C:2]1[C:3]([C:10]2[CH:15]=[CH:14][C:13]([C:16]([O:18]C)=[O:17])=[CH:12][C:11]=2[C:20]([O:22][CH3:23])=[O:21])=[CH:4][C:5]([O:8][CH3:9])=[N:6][CH:7]=1.[OH-].[K+].Cl>C1COCC1.CO>[F:1][C:2]1[C:3]([C:10]2[CH:15]=[CH:14][C:13]([C:16]([OH:18])=[O:17])=[CH:12][C:11]=2[C:20]([O:22][CH3:23])=[O:21])=[CH:4][C:5]([O:8][CH3:9])=[N:6][CH:7]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 57706068Dimethyl 4-(5-fluoro-2-(methyloxy)-4-pyridinyl)-1,3-benzenedicarboxylate

생성물 1

HCID 574675964-(5-Fluoro-2-(methyloxy)-4-pyridinyl)-3-((methyloxy)carbonyl)benzoic acid수율 100%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 83.21A (0.860 g, 2.7 mmol) in THF (7.00 mL) and MeOH (7.00 mL) at 0° C. was added potassium hydroxide (1.5 mL, 3.0 mmol) slowly to maintain the temperature below 6° C. The reaction mixture was allowed to warm to room temperature and stirred for 17 hours. After which, the reaction was acidified with 1N HCl and extracted three times with EtOAc. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure to yield 83.21B as a colorless solid (0.82 g, 100% yield).

후처리

  1. temperatureto maintain the temperature below 6° C
  2. extractionextracted three times with EtOAc
  3. dry with materialAfter drying over anhydrous magnesium sulfate
  4. filtrationfiltering
  5. customthe organic solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-0811189dcd3b4d11bbcada8cf4e47215
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030354B2

반응 노트

불러오는 중…