Water → HCID 20137755, Verbindung

HRID 1982100Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1982100
[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.C[O:20][C:21](=O)[NH:22][C:23]1[N:28]=[C:27]([O:29][CH3:30])[N:26]=[C:25]([O:31][CH3:32])[N:24]=1.O>C(Cl)Cl.Cl.C(O)(=O)C>[CH3:30][O:29][C:27]1[N:26]=[C:25]([O:31][CH3:32])[N:24]=[C:23]([NH:22][C:21]([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:20])[N:28]=1

Komponenten

8

Edukt 4

HCID 962WaterHCID 12803256Methyl (4,6-dimethoxy-1,3,5-triazin-2-yl)carbamateHCID 16682925TrimethylaluminumHCID 201377482,3-Dihydro-1,4-benzodithiine-5-sulfonamide

Produkt 1

HCID 20137755HCID 20137755, 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 16, 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[4,6-Dimethoxy-1,3,5-triazin-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 an appropriate organic solvent 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 an appropriate organic solvent
  10. customgives a solid

Quellen und Nachweise

ORD-Eintrag
ord-2ab4eb87e0fe4dfe8014ddbb9e1857b6
Quelldatensatz
uspto-grants-1986_06
Patentnummer
US04595407

Notizen zur Reaktion

Wird geladen…