1-Methyluracil → (+/-)-1-Methyl-5-(2-methyl-7-n-propyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-2,4-(1H,3H)-pyrimidinedione

HRID 324468

Reaktionsgleichung

Reaktionsgleichung von HRID 324468
[CH3:1][N:2]1[CH:9]=[CH:8][C:6](=[O:7])[NH:5][C:3]1=[O:4].[CH3:10][C:11]1[S:12][C:13]2[CH:20]=[CH:19][C:18]3[CH:21]=[C:22]([CH2:25][CH2:26][CH3:27])[CH:23]=[CH:24][C:17]=3[CH:16](O)[C:14]=2[N:15]=1>C(O)(=O)C>[CH3:1][N:2]1[CH:9]=[C:8]([CH:16]2[C:14]3[N:15]=[C:11]([CH3:10])[S:12][C:13]=3[CH:20]=[CH:19][C:18]3[CH:21]=[C:22]([CH2:25][CH2:26][CH3:27])[CH:23]=[CH:24][C:17]2=3)[C:6](=[O:7])[NH:5][C:3]1=[O:4]

Komponenten

4

Edukt 2

HCID 120091-MethyluracilHCID 70112533(+/-)-2-Methyl-7-n-propyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-ol

Produkt 1

HCID 70115254(+/-)-1-Methyl-5-(2-methyl-7-n-propyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-2,4-(1H,3H)-pyrimidinedione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A mixture of the 1-methyluracil (0.5 g) and the product from step (xi) in acetic acid (50 ml) was heated at reflux 2 h. The solvent was removed under reduced pressure and the residue partitioned between ethyl acetate/water. The organic layer collected and dried over MgSO4. The solvent evaporated and the crude product purified by flash chromatography eluting with ethyl acetate.

Aufarbeitung

  1. temperatureat reflux 2 h
  2. customThe solvent was removed under reduced pressure
  3. customthe residue partitioned between ethyl acetate/water
  4. customThe organic layer collected
  5. dry with materialdried over MgSO4
  6. customThe solvent evaporated
  7. customthe crude product purified by flash chromatography
  8. washeluting with ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-f8bee6b99aaa4484b4d79496ff0e3701
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06218376B1

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