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Pyridine → Methyl 3-[(6-chloro-3-methyl-pyridine-2-carbonyl)amino]-2,4-dimethyl-benzoate

HRID 1427122
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1427122
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=O)[C:5]([CH3:11])=[CH:4][CH:3]=1.[C:12](Cl)(=O)[C:13](Cl)=O.NC1(C)C=C(C)C=C([C:22]([O:24][CH3:25])=[O:23])C1.[N:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.[CH2:37]1COCC1>C(Cl)Cl.CN(C)C1C=CN=CC=1.CN(C=O)C>[Cl:1][C:2]1[N:7]=[C:6]([C:8]([NH:31][C:36]2[C:12]([CH3:13])=[C:32]([CH:33]=[CH:34][C:35]=2[CH3:37])[C:22]([O:24][CH3:25])=[O:23])=[O:10])[C:5]([CH3:11])=[CH:4][CH:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 5

HCID 1049PyridineHCID 8028TetrahydrofuranHCID 65578Oxalyl chlorideHCID 469414706-Chloro-3-methylpyridine-2-carboxylic acidHCID 86707353Methyl 3-amino-3,5-dimethylbenzoate

Produkt 1

HCID 86707343Methyl 3-[(6-chloro-3-methyl-pyridine-2-carbonyl)amino]-2,4-dimethyl-benzoate
Ausbeute 73 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 6228DimethylformamideKatalysatorHCID 142844-(Dimethylamino)pyridineKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 6-chloro-3-methyl-pyridine-2-carboxylic acid (465 mg, 2.71 mmol) in THF (5 ml), CH2Cl2 (5 ml) and DMF (0.01 ml, 129.33 μmoles) is added dropwise oxalyl chloride (0.3 ml, 3.46 mmoles) at 0° C. and the reaction mixture is slowly allowed to warm to ambient temperature. After 2 hours, the solvent is removed under reduced pressure. To the residue CH2Cl2 (20 ml) is added and reaction mixture is cooled to 0° C., then methyl 3-amino-3,5-dimethylbenzoate (490 mg, 2.73 mmol) is added followed by N,N-dimethylpyridin-4-amine (15 mg, 122.78 μmoles) and pyridine (0.66 ml, 8.16 mmoles). The cooling bath is removed and the clear solution is allowed to warm to ambient temperature. After 1.5 hours, the solvent is removed and the reaction mixture is diluted with ethyl acetate and washed with 0.5N HCl, saturated solution of sodium bicarbonate, and brine. The organic layers are combined and dried over anhydrous Na2SO4, filtered, and concentrated under reduced pressure to give the title compound as a light yellow solid (664 mg, 73%). Mass spectrum (m/z): 333.2 (M+1).

Aufarbeitung

  1. customthe solvent is removed under reduced pressure
  2. additionTo the residue CH2Cl2 (20 ml) is added
  3. customreaction mixture
  4. temperatureis cooled to 0° C.
  5. customThe cooling bath is removed
  6. temperatureto warm to ambient temperature
  7. waitAfter 1.5 hours
  8. customthe solvent is removed
  9. additionthe reaction mixture is diluted with ethyl acetate
  10. washwashed with 0.5N HCl, saturated solution of sodium bicarbonate, and brine
  11. dry with materialdried over anhydrous Na2SO4
  12. filtrationfiltered
  13. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-b2c75b51a33f467aa7c941e8efe34de9
Quelldatensatz
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08933098B2

Notizen zur Reaktion

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