Benzoyl chloride, 3-bromo- → 6-(3-bromo-benzoyl)-4-methyl-3H-benzoxazol-2-one

HRID 469321Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 469321
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5](Cl)=[O:6].[CH3:11][C:12]1[C:17]2[NH:18][C:19](=[O:21])[O:20][C:16]=2[CH:15]=[CH:14][CH:13]=1.[Cl-].[Cl-].[Cl-].[Al+3]>>[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([C:14]1[CH:13]=[C:12]([CH3:11])[C:17]2[NH:18][C:19](=[O:21])[O:20][C:16]=2[CH:15]=1)=[O:6]

Komponenten

4

Edukt 3

HCID 74377Benzoyl chloride, 3-bromo-HCID 6451240Aluminum(III) ChlorideHCID 127093364-Methyl-3H-benzooxazol-2-one

Produkt 1

HCID 581811686-(3-bromo-benzoyl)-4-methyl-3H-benzoxazol-2-one

Versuchsvorschrift

2.08 g (9.48 mmol) 3-bromo-benzoic acid chloride, 1.41 g (9.48 mmol) 4-methyl-3H-benzoxazol-2-one and 5.33 g (40.0 mmol) aluminium trichloride were heated to 125° C. with stirring for 1.5 h. Then the mixture was mixed with ice water and the grease precipitated was separated from the solvent by decanting. The residue was dissolved in EtOAc, evaporated down and a little MeOH was triturated. The precipitate formed was suction filtered, washed with diethyl ether and dried i. vac.

Aufarbeitung

  1. customthe grease precipitated
  2. customwas separated from the solvent
  3. customby decanting
  4. dissolutionThe residue was dissolved in EtOAc
  5. customevaporated down
  6. customa little MeOH was triturated
  7. customThe precipitate formed
  8. filtrationfiltered
  9. washwashed with diethyl ether
  10. customdried i

Quellen und Nachweise

ORD-Eintrag
ord-791f12d87530497d82841e3bc08eb5f5
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08629137B2

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