Phosphorus oxychloride → HCID 86659539, 화합물

HRID 1256941노트

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HRID 1256941 반응식
[F:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[C:8](=O)[NH:7][CH:6]=[C:5]2[C:13]([O:15][CH3:16])=[O:14].P(Cl)(Cl)([Cl:19])=O>>[Cl:19][C:8]1[C:9]2[C:4](=[CH:3][C:2]([F:1])=[CH:11][CH:10]=2)[C:5]([C:13]([O:15][CH3:16])=[O:14])=[CH:6][N:7]=1

참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 53429435Methyl 6-fluoro-1-oxo-1,2-dihydroisoquinoline-4-carboxylate

생성물 1

HCID 86659539HCID 86659539, 화합물

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온도
100 °C

실험 절차

To methyl 6-fluoro-1oxo-1,2-dihydroisoquinoline-4-carboxylate (756 mg), phosphoryl chloride (5 ml) was added, and the mixture was stirred at 100° C. for one hour. The resulting solution was returned to room temperature, and evaporated under reduced pressure to remove the solvent. To the resulting crude product, saturated sodium bicarbonate water was added, followed by extraction with ethyl acetate. The organic layer was washed with a saturated saline solution, dried over anhydrous magnesium sulfate, and evaporated under reduced pressure to remove the solvent to give methyl 1-chloro-6-fluoroisoquinoline-4-carboxylate (792 mg) as a brown solid.

후처리

  1. customwas returned to room temperature
  2. customevaporated under reduced pressure
  3. customto remove the solvent
  4. additionTo the resulting crude product, saturated sodium bicarbonate water was added
  5. extractionfollowed by extraction with ethyl acetate
  6. washThe organic layer was washed with a saturated saline solution
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customevaporated under reduced pressure
  9. customto remove the solvent

출처 및 근거

ORD 기록
ord-046ac44e3bdc4c3d9c26c46413a558c1
출처 데이터셋
uspto-grants-2013_06
특허 번호
US08461329B2

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