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Oxalyl chloride → N-(6-chloro-2-fluoro-3-hydroxy-phenyl)-2-fluoro-5-(3-fluorophenyl)benzamide

HRID 1771641
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HRID 1771641 반응식
[F:1][C:2]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[CH:12]=2)=[CH:7][C:3]=1[C:4]([OH:6])=O.C(Cl)(C(Cl)=O)=O.[NH2:24][C:25]1[C:26]([F:33])=[C:27]([OH:32])[CH:28]=[CH:29][C:30]=1[Cl:31].C([O-])(O)=O.[Na+]>C(Cl)Cl.C1COCC1.CN(C=O)C>[Cl:31][C:30]1[C:25]([NH:24][C:4](=[O:6])[C:3]2[CH:7]=[C:8]([C:11]3[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[CH:12]=3)[CH:9]=[CH:10][C:2]=2[F:1])=[C:26]([F:33])[C:27]([OH:32])=[CH:28][CH:29]=1
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참가 물질

8

반응물 4

HCID 65578Oxalyl chlorideHCID 516892Sodium BicarbonateHCID 463123323',4-Difluoro-[1,1'-biphenyl]-3-carboxylic acidHCID 847644353-Amino-4-chloro-2-fluorophenol

생성물 1

HCID 89445317N-(6-chloro-2-fluoro-3-hydroxy-phenyl)-2-fluoro-5-(3-fluorophenyl)benzamide수율 26%

시약·촉매·용매 3

HCID 6228
Dimethylformamide
용매
HCID 6344Dichloromethane용매
HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

To a mixture of 2-fluoro-5-(3-fluorophenyl)benzoic acid (intermediate III(a)) (478 mg, 2.04 mmol, 1.0 eq) and (COCl)2 (777 mg, 6.13 mmol, 3.0 eq) in DCM (20 mL) was added DMF (0.3 mL). The reaction mixture was stirred at 0° C. for 1 h, then the solvent removed in vacuo. The residue obtained was dissolved in THF (20 mL) and added dropwise to a solution of 3-amino-4-chloro-2-fluoro-phenol (intermediate X(d)) (330 mg, 2.04 mmol, 1.0 eq) and NaHCO3 (515 mg, 6.13 mmol, 3.0 eq) in THF (20 mL). After the addition, the reaction mixture was stirred at room temperature for 30 min. The THF was evaporated in vacuo and the aqueous solution adjusted to pH 3 by addition of 1M HCl. The mixture was extracted with EtOAc and the combined organic extracts were dried (Na2SO4), filtered and evaporated in vacuo. The residue was purified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:1) to give the title compound as a yellow solid (200 mg, 26%).

후처리

  1. customthe solvent removed in vacuo
  2. customThe residue obtained
  3. additionAfter the addition
  4. stirringthe reaction mixture was stirred at room temperature for 30 min
  5. customThe THF was evaporated in vacuo
  6. additionthe aqueous solution adjusted to pH 3 by addition of 1M HCl
  7. extractionThe mixture was extracted with EtOAc
  8. dry with materialthe combined organic extracts were dried (Na2SO4)
  9. filtrationfiltered
  10. customevaporated in vacuo
  11. customThe residue was purified by column chromatography (EtOAc:petroleum ether, 0:1 to 1:1)

출처 및 근거

ORD 기록
ord-6f00c1704a3f4d0b9b9c518e8175e4f4
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09249085B2

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