3-Fluoro-2-hydroxybenzoic acid → Methyl 3-fluoro-2-hydroxybenzoate

HRID 1390922

반응식

HRID 1390922 반응식
[F:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:4]([C:5]([OH:7])=[O:6])[C:3]=1[OH:11].B(F)(F)F.CO.[C:18](=O)(O)[O-].[Na+]>CO>[CH3:18][O:6][C:5](=[O:7])[C:4]1[C:3](=[C:2]([F:1])[CH:10]=[CH:9][CH:8]=1)[OH:11]

참가 물질

5

반응물 3

HCID 2687243-Fluoro-2-hydroxybenzoic acidHCID 516892Sodium BicarbonateHCID 11062313373-57-9

생성물 1

HCID 573875Methyl 3-fluoro-2-hydroxybenzoate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A 15.6 g (0.10 mole) portion of 3-fluorosalicylic acid was dissolved in a 100 ml portion of absolute methanol. A 22 ml portion of borontrifluoride-methanol reagent (2 equivalents, 51% BF3) was added and the reaction allowed to reflux for about six hours. The reaction mixture was cooled and added carefully to a saturated solution of sodium bicarbonate. The resulting mixture was then extracted with ether, the ether layer dried over magnesium sulfate and evaporated in vacuo. The oil obtained was crystallized from methanol. The methyl-3-fluorosalicylate obtained had a melting point of 94°-5° C.

후처리

  1. temperatureto reflux for about six hours
  2. temperatureThe reaction mixture was cooled
  3. extractionThe resulting mixture was then extracted with ether
  4. dry with materialthe ether layer dried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe oil obtained
  7. customwas crystallized from methanol

출처 및 근거

ORD 기록
ord-67d48203d25e4475b44bc5781c643097
출처 데이터셋
uspto-grants-1979_02
특허 번호
US04140769

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