Acetic Anhydride → N-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7H,8H-pyrido[2,3-d]pyrimidin-2-yl]acetamide

HRID 53624

Reaktionsgleichung

Reaktionsgleichung von HRID 53624
[NH2:1][C:2]1[N:3]=[CH:4][C:5]2[CH:11]=[C:10]([C:12]3[C:17]([Cl:18])=[CH:16][CH:15]=[CH:14][C:13]=3[Cl:19])[C:9](=[O:20])[N:8]([CH3:21])[C:6]=2[N:7]=1.[C:22](OC(=O)C)(=[O:24])[CH3:23]>>[Cl:18][C:17]1[CH:16]=[CH:15][CH:14]=[C:13]([Cl:19])[C:12]=1[C:10]1[C:9](=[O:20])[N:8]([CH3:21])[C:6]2[N:7]=[C:2]([NH:1][C:22](=[O:24])[CH3:23])[N:3]=[CH:4][C:5]=2[CH:11]=1

Komponenten

3

Edukt 2

HCID 7918Acetic AnhydrideHCID 53278642-amino-6-(2,6-dichlorophenyl)-8-methyl-7H,8H-pyrido[2,3-d]pyrimidin-7-one

Produkt 1

HCID 5327865N-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7H,8H-pyrido[2,3-d]pyrimidin-2-yl]acetamide

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

A mixture of 64.2 mg (0.20 mmol) of 2-amino-6-(2,6-dichlorophenyl)-8-methyl-pyrido[2,3-d]pyrimidin-7(8H)-one (from Example 12) and 1 mL of acetic anhydride was heated to reflux. The resulting solution was maintained at reflux for 20 minutes and concentrated at atmospheric pressure to about 0.25 mL volume. The solution was cooled to 25° C. and diluted with diethyl ether (1 mL). The separated crystals were filtered and washed with diethyl ether to provide N-[6-(2,6-dichlorophenyl)-8-methyl-7-oxo-7,8-dihydro-pyrido[2,3-d]pyrimidin-2-yl]acetamide, wt 44.0 mg; mp 258°-260° C.; MS (CI) 363 (M+ +1).

Aufarbeitung

  1. temperaturewas heated to reflux
  2. temperatureThe resulting solution was maintained
  3. temperatureat reflux for 20 minutes
  4. concentrationconcentrated at atmospheric pressure to about 0.25 mL volume
  5. additiondiluted with diethyl ether (1 mL)
  6. filtrationThe separated crystals were filtered
  7. washwashed with diethyl ether

Quellen und Nachweise

ORD-Eintrag
ord-26a020e1e80a4d4c857431a3c9c2b02f
Quelldatensatz
uspto-grants-1997_04
Patentnummer
US05620981

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