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2,6-Dichloroaniline → 3-[4,6-dibromo-2-(2-chloro-4-fluorophenyl)pyridin-3-yl]-N-(2,6-dichlorophenyl)propanamide

HRID 394178
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HRID 394178 반응식
[Br:1][C:2]1[CH:7]=[C:6]([Br:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=2[Cl:16])[C:3]=1[CH2:17][CH2:18][C:19]([O:21]C(C)(C)C)=O.C[Si](C=[N+]=[N-])(C)C.[Cl:33][C:34]1[CH:40]=[CH:39][CH:38]=[C:37]([Cl:41])[C:35]=1[NH2:36].C[Al](C)C.C([O-])(=O)C(C(C([O-])=O)O)O.[Na+].[K+]>FC(F)(F)C(O)=O.C(Cl)Cl.O.C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[C:6]([Br:8])[N:5]=[C:4]([C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][C:10]=2[Cl:16])[C:3]=1[CH2:17][CH2:18][C:19]([NH:36][C:35]1[C:34]([Cl:33])=[CH:40][CH:39]=[CH:38][C:37]=1[Cl:41])=[O:21]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 5

HCID 118462,6-DichloroanilineHCID 167693TrimethylsilyldiazomethaneHCID 9855836Potassium sodium tartarateHCID 16682925TrimethylaluminumHCID 22647943Tert-butyl 3-[4,6-dibromo-2-(2-chloro-4-fluorophenyl)pyridin-3-yl]propanoate

생성물 1

HCID 22647911
3-[4,6-dibromo-2-(2-chloro-4-fluorophenyl)pyridin-3-yl]-N-(2,6-dichlorophenyl)propanamide

시약·촉매·용매 5

HCID 6422Trifluoroacetic acid촉매HCID 962Water용매HCID 1140Toluene용매2회HCID 6344Dichloromethane용매3회HCID 6422Trifluoroacetic acid용매

실험 절차

tert-butyl 3-[-4,6-dibromo-2-(2-chloro-4-fluorophenyl)pyridin-3-yl]propanoate (3.42 g, 6.93 mmol) was dissolved in 12 mL of trifluoroacetic acid and stirred at rt for 0.75 h. 30 mL of toluene was added and the resulting mixture was concentrated under reduced pressure. The resulting solid was dissolved in 50 mL of benzene and 5 mL of methanol. A 2M solution of (trimethylsilyl)diazomethane in hexanes (4.16 mL, 8.32 mmol) was added dropwise and the reaction mixture was stirred for 30 min. 2 drops of trifluoroacetic acid were added and the solvent was removed under reduced pressure. The resulting methyl ester was dissolved in 12 mL of CH2Cl2. To 2,6-dichloroaniline (2.25 g, 13.9 mmol) in 36 mL of CH2Cl2 was added dropwise a 2M solution of trimethylaluminum in toluene (7.0 mL, 13.9 mmol) and the mixture was stirred for 15 min. Then the methyl ester solution in CH2Cl2 was added and the resulting mixture was stirred at rt overnight. 24 mL of water was added very carefully followed by 12 mL of an aqueous 1M solution of potassium sodium tartarate and 24 mL of CH2Cl2. The mixture was stirred vigorously for 1 h and then filtered. The filtered solids were dissolved with CH2Cl2, washed with brine, dried over Na2SO4, and concentrated under reduced pressure to give one pure crop. The filtrate was separated, washed with brine, dried over Na2SO4, and concentrated under reduced pressure. The residue was triturated with hot ethanol to give a second pure crop. The two crops were combined to give the 3-[4,6-dibromo-2-(2-chloro-4-fluorophenyl)pyridin-3-yl]-N-(2,6-dichlorophenyl)propanamide as a white solid.

후처리

  1. concentrationthe resulting mixture was concentrated under reduced pressure
  2. dissolutionThe resulting solid was dissolved in 50 mL of benzene
  3. stirringthe reaction mixture was stirred for 30 min
  4. customthe solvent was removed under reduced pressure
  5. dissolutionThe resulting methyl ester was dissolved in 12 mL of CH2Cl2
  6. stirringthe mixture was stirred for 15 min
  7. stirringthe resulting mixture was stirred at rt overnight
  8. stirringThe mixture was stirred vigorously for 1 h
  9. filtrationfiltered
  10. dissolutionThe filtered solids were dissolved with CH2Cl2
  11. washwashed with brine
  12. dry with materialdried over Na2SO4
  13. concentrationconcentrated under reduced pressure
  14. customto give one pure crop
  15. customThe filtrate was separated
  16. washwashed with brine
  17. dry with materialdried over Na2SO4
  18. concentrationconcentrated under reduced pressure
  19. customThe residue was triturated with hot ethanol
  20. customto give a second pure crop

출처 및 근거

ORD 기록
ord-6e57340edd55485ebed4f0adcdd6737f
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06809199B2

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