Isopropanol → (1-Methylethyl) [3-[[(4-methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]aminosulfonyl]phenyl]carbamate

HRID 1262796

Reaktionsgleichung

Reaktionsgleichung von HRID 1262796
[N:1]([C:4]1[CH:5]=[C:6]([S:10]([N:13]=[C:14]=[O:15])(=[O:12])=[O:11])[CH:7]=[CH:8][CH:9]=1)=[C:2]=[O:3].[NH2:16][C:17]1[N:22]=[C:21]([O:23][CH3:24])[CH:20]=[C:19]([CH3:25])[N:18]=1.[CH3:26][CH:27]([OH:29])[CH3:28]>C(Cl)Cl>[CH3:24][O:23][C:21]1[CH:20]=[C:19]([CH3:25])[N:18]=[C:17]([NH:16][C:14]([NH:13][S:10]([C:6]2[CH:5]=[C:4]([NH:1][C:2](=[O:3])[O:29][CH:27]([CH3:28])[CH3:26])[CH:9]=[CH:8][CH:7]=2)(=[O:11])=[O:12])=[O:15])[N:22]=1

Komponenten

5

Edukt 3

HCID 3776IsopropanolHCID 5872364-Methoxy-6-methylpyrimidin-2-amineHCID 13138205m-Isocyanatobenzenesulfonyl isocyanate

Produkt 1

HCID 13138206(1-Methylethyl) [3-[[(4-methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]aminosulfonyl]phenyl]carbamate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To an anhydrous solution of 2.3 g of m-isocyanatobenzenesulfonyl isocyanate in 50 ml of methylene chloride was added in small portions 1.4 g of 2-amino-4-methoxy-6-methylpyrimidine. Efficient stirring was maintained during the addition and for three additional hours. The intermediate thus obtained, 3-isocyanto-N-[(4-methoxy-6-methylpyrimidin-2-yl)aminocarbonyl]benzenesulfonamide, was reacted further by adding one gram of 2 -propanol and stirring the resultant mixture for an additional sixteen hours. Filtration of the reaction mixture and evaporation of the filtrate yielded the desired product melting at 173°-180°.

Aufarbeitung

  1. temperaturewas maintained during the addition and for three additional hours
  2. customThe intermediate thus obtained
  3. filtrationFiltration of the reaction mixture and evaporation of the filtrate

Quellen und Nachweise

ORD-Eintrag
ord-9ece9c9fc41140b8b3a41f01c41e39a5
Quelldatensatz
uspto-grants-1984_06
Patentnummer
US04453971

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