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Methanol → Methyl 2-chloro-3-fluoropyridine-4-carboxylate

HRID 1180244
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HRID 1180244 반응식
[Cl:1][C:2]1[C:3]([F:11])=[C:4]([CH:8]=[CH:9][N:10]=1)[C:5]([OH:7])=[O:6].[CH3:12]O>S(Cl)(Cl)=O.ClCCl>[CH3:12][O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][N:10]=[C:2]([Cl:1])[C:3]=1[F:11]
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참가 물질

5

반응물 2

HCID 887MethanolHCID 27828122-Chloro-3-fluoropyridine-4-carboxylic acid

생성물 1

HCID 24820381Methyl 2-chloro-3-fluoropyridine-4-carboxylate수율 93.2%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 24386Thionyl Chloride용매

실험 절차

2-Chloro-3-fluoroisonicotinic acid (3.30 g, 18.8 mmol) was suspended in thionyl chloride (40 ml) and heated under reflux for 2.5 h. The solvent was evaporated and the residue dried by means of azeotropic removal of water with toluene (100 ml) to afford a pale yellow oil. The oil was dissolved in dichloromethane (20 ml) and cooled to 0° C. before methanol (2.42 g, 75.3 mmol) was added dropwise to the solution over 15 min. On complete addition the mixture was allowed to warm to ambient temperature and stirred for 18 h. The solvent was evaporated and the mixture partitioned between water (75 ml) and dichloromethane (100 ml). The aqueous phase was extracted further with dichloromethane (100 ml), the organic layers were combined, washed with brine (75 ml), dried over anhydrous sodium sulphate, filtered and evaporated to give 2-chloro-3-fluoroisonicotinic acid methyl ester (3.32 g, 93%) as a pale yellow solid: δH (360 MHz, CDCl3) 3.99 (3H, s), 7.70 (1H, dd, J 5 and 5), 8.31 (1H, d, J 5).

후처리

  1. temperatureheated
  2. temperatureunder reflux for 2.5 h
  3. customThe solvent was evaporated
  4. dry with materialthe residue dried by means of azeotropic removal of water with toluene (100 ml)
  5. customto afford a pale yellow oil
  6. additionwas added dropwise to the solution over 15 min
  7. additionOn complete addition the mixture
  8. customThe solvent was evaporated
  9. customthe mixture partitioned between water (75 ml) and dichloromethane (100 ml)
  10. extractionThe aqueous phase was extracted further with dichloromethane (100 ml)
  11. washwashed with brine (75 ml)
  12. dry with materialdried over anhydrous sodium sulphate
  13. filtrationfiltered
  14. customevaporated

출처 및 근거

ORD 기록
ord-7ddd90cc31fb48abb7e16c882e98708c
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07279580B2

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