Water → HCID 20137751, Verbindung

HRID 2164210Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2164210
[S:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([S:11]([NH2:14])(=[O:13])=[O:12])[C:5]=2[S:4][CH2:3][CH2:2]1.C[Al](C)C.[CH3:19][O:20][C:21]1[CH:26]=[C:25]([CH3:27])[N:24]=[C:23]([NH:28][C:29](=O)[O:30]C)[N:22]=1.O>C(Cl)Cl.Cl.C(O)(=O)C>[CH3:19][O:20][C:21]1[CH:26]=[C:25]([CH3:27])[N:24]=[C:23]([NH:28][C:29]([NH:14][S:11]([C:10]2[C:5]3[S:4][CH2:3][CH2:2][S:1][C:6]=3[CH:7]=[CH:8][CH:9]=2)(=[O:12])=[O:13])=[O:30])[N:22]=1

Komponenten

8

Edukt 4

HCID 962WaterHCID 13072161Methyl (4-methoxy-6-methylpyrimidin-2-yl)carbamateHCID 16682925TrimethylaluminumHCID 201377482,3-Dihydro-1,4-benzodithiine-5-sulfonamide

Produkt 1

HCID 20137751HCID 20137751, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 313Hydrochloric AcidKatalysatorHCID 176Acetic AcidLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a solution of 2.5 g 1,4-benzodithian-5-sulfonamide, prepared in Example 18, in 50 ml methylene chloride at ambient temperature under nitrogen is added 5.5 ml trimethylaluminum (2M in toluene). After stirring 15 minutes at ambient temperature 2.0 g of methyl [4-methoxy-6-methylpyrimidin-2-yl]carbamate, prepared according to the procedure of Example 3, is added and the reaction mixture is heated at reflux for 16 hours. The reaction mixture is cooled to ambient temperature and 75 ml water, 10 ml glacial acetic acid, and 10 drops hydrochloric acid are sequentially added. The organic phase is separated, dried, and the solvent removed under reduced pressure to give an oil. Crystallization of the oil from n-butyl chloride/ether gives a solid.

Aufarbeitung

  1. customprepared
  2. additionis added
  3. temperaturethe reaction mixture is heated
  4. temperatureat reflux for 16 hours
  5. customThe organic phase is separated
  6. customdried
  7. customthe solvent removed under reduced pressure
  8. customto give an oil
  9. customCrystallization of the oil from n-butyl chloride/ether
  10. customgives a solid

Quellen und Nachweise

ORD-Eintrag
ord-4e6fb41d7a224b61b95089c0218a07d5
Quelldatensatz
uspto-grants-1985_03
Patentnummer
US04502882

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