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Cesium carbonate → 5-chloro-4-(3-ethoxyphenoxy)-2-fluoro-N-(methylsulfonyl)benzamide

HRID 2359260
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HRID 2359260 반응식
[Cl:1][C:2]1[C:3](F)=[CH:4][C:5]([F:12])=[C:6]([CH:11]=1)[C:7]([O:9]C)=O.[CH2:14]([O:16][C:17]1[CH:18]=[C:19]([OH:23])[CH:20]=[CH:21][CH:22]=1)[CH3:15].C(=O)([O-])[O-].[Cs+].[Cs+].[CH3:30][S:31]([NH2:34])(=[O:33])=[O:32].CCN=C=NCCCN(C)C.Cl>CN(C)C=O.CN(C)C1C=CN=CC=1.ClCCl.C(#N)C.O>[Cl:1][C:2]1[C:3]([O:23][C:19]2[CH:20]=[CH:21][CH:22]=[C:17]([O:16][CH2:14][CH3:15])[CH:18]=2)=[CH:4][C:5]([F:12])=[C:6]([CH:11]=1)[C:7]([NH:34][S:31]([CH3:30])(=[O:33])=[O:32])=[O:9]
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참가 물질

10

반응물 5

HCID 10796Cesium carbonateHCID 693063-EthoxyphenolHCID 72879MethanesulfonamideHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 58042369Methyl 5-chloro-2,4-difluorobenzoate

생성물 1

HCID 565925365-chloro-4-(3-ethoxyphenoxy)-2-fluoro-N-(methylsulfonyl)benzamide
수율 12.8%

시약·촉매·용매 4

HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매HCID 18373917Acetonitrile--water (1/1)용매

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온도
120 °C

실험 절차

To solution of methyl 5-chloro-2,4-difluorobenzoate (25.9 mg, 0.125 mmol) and 3-ethoxyphenol (17.3 mg, 0.125 mmol) in dimethyl formamide (0.5 mL) was added cesium carbonate (82 mg, 0.25 mmol), the mixture was shaken at 120° C. for 16 hours, filtered and evaporated in vacuo. Water (1 mL) was added and extracted with ethyl acetate (3×1 mL), the combined organic layers were dried over sodium sulphate, filtered and evaporated in vacuo. The residue was dissolved in THF (0.7 mL) and to this solution was added a 1M aqueous solution of lithium hydroxide (0.7 mL) and the mixture was shaken at 30° C. for 16 hours. The reaction mixture was evaporated in vacuo, a 1M aqueous solution of hydrochloric acid (0.7 mL) was added and extracted with ethyl acetate (3×1 mL). The combined organic layers were dried over anhydrous sodium sulphate, filtered and evaporated in vacuo. To this residue was added methanesulfonamide (28.6 mg, 0.300 mmol) and a solution of 4-dimethylaminopyridine (24.4 mg, 0.200 mmol) and EDCl (38.3 mg, 0.200 mmol) in dichloromethane (1 mL), the solution was shaken at 30° C. for 16 hours and evaporated in vacuo. The crude product was purified on a HPLC column (Sepax BR-C18 100*21.2 mm*5 μm, acetonitrile-water (0.1% trifluoroacetic acid) gradient to yield 6.2 mg (16 μmol) 5-chloro-4-(3-ethoxyphenoxy)-2-fluoro-N-(methylsulfonyl)benzamide.

후처리

  1. filtrationfiltered
  2. customevaporated in vacuo
  3. additionWater (1 mL) was added
  4. extractionextracted with ethyl acetate (3×1 mL)
  5. dry with materialthe combined organic layers were dried over sodium sulphate
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. dissolutionThe residue was dissolved in THF (0.7 mL) and to this solution
  9. additionwas added a 1M aqueous solution of lithium hydroxide (0.7 mL)
  10. stirringthe mixture was shaken at 30° C. for 16 hours
  11. customThe reaction mixture was evaporated in vacuo
  12. additiona 1M aqueous solution of hydrochloric acid (0.7 mL) was added
  13. extractionextracted with ethyl acetate (3×1 mL)
  14. dry with materialThe combined organic layers were dried over anhydrous sodium sulphate
  15. filtrationfiltered
  16. customevaporated in vacuo
  17. customevaporated in vacuo
  18. customThe crude product was purified on a HPLC column (Sepax

출처 및 근거

ORD 기록
ord-85d40699507e472f859356d72200a774
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08685977B2

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