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Hydrochloric Acid → 6-[2-(2-chloro-5-methoxy-phenyl)-acetyl]-4-methyl-4H-benzo[1,4]oxazin-3-one

HRID 2096712
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2096712
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[CH2:10][C:11]([OH:13])=O.C(Cl)(=O)C(Cl)=O.[CH3:20][N:21]1[C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=2[O:24][CH2:23][C:22]1=[O:31].[Al+3].[Cl-].[Cl-].[Cl-].Cl>O1CCCC1.CN(C)C=O.ClCCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][C:3]=1[CH2:10][C:11]([C:28]1[CH:29]=[CH:30][C:25]2[O:24][CH2:23][C:22](=[O:31])[N:21]([CH3:20])[C:26]=2[CH:27]=1)=[O:13]
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Komponenten

9

Edukt 5

HCID 313Hydrochloric AcidHCID 65578Oxalyl chlorideHCID 890322H-1,4-Benzoxazin-3(4H)-one,4-methyl-HCID 6451240Aluminum(III) ChlorideHCID 153659582-(2-Chloro-5-methoxyphenyl)acetic acid

Produkt 1

HCID 666972226-[2-(2-chloro-5-methoxy-phenyl)-acetyl]-4-methyl-4H-benzo[1,4]oxazin-3-one
Ausbeute 92,8 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6228DimethylformamideKatalysatorHCID 111,2-DichloroethaneLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of (2-chloro-5-methoxy-phenyl)-acetic acid (1 g) in tetrahydrofuran (20 ml) were added N,N-dimethylformamide (2 drops) and oxalylchloride (1.03 g). The mixture was stirred overnight at room temperature. The solvent was evaporated; toluene was added and again evaporated. The residue was dried under high vacuum to give the crude acid chloride. To a cooled solution (ice bath) of 4-methyl-2H-1,4-benzoxazin-3(4H)-one (830 mg) in 1,2-dichloroethane (5 ml) was added AlCl3 (1.99 g). The mixture was stirred for 10 min and a solution of the acid chloride in 1,2-dichloroethane (5 ml) was added dropwise. The mixture was stirred at 0° C. for 4.5 h. The mixture was poured into ice water and hydrochloric acid and extracted with dichloromethane. The organic phase was dried (MgSO4), filtered and concentrated. The product was purified by chromatography (SiO2, cyclohexane/EtOAc 1:0=>0:1) to give the title compound (1.6 g) as an off-white solid. MS (m/e)=346.1 [M+H+].

Aufarbeitung

  1. customThe solvent was evaporated
  2. additiontoluene was added
  3. customagain evaporated
  4. customThe residue was dried under high vacuum
  5. customto give the crude acid chloride
  6. stirringThe mixture was stirred for 10 min
  7. stirringThe mixture was stirred at 0° C. for 4.5 h
  8. extractionextracted with dichloromethane
  9. dry with materialThe organic phase was dried (MgSO4)
  10. filtrationfiltered
  11. concentrationconcentrated
  12. customThe product was purified by chromatography (SiO2, cyclohexane/EtOAc 1:0=>0:1)

Quellen und Nachweise

ORD-Eintrag
ord-bc28f390f0f54ba4ab1c9396df5437fd
Quelldatensatz
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08450313B2

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