Reaktion #429152

Reaktionsgleichung

Hunig base

bis-(2-oxo-3-oxazolidinyl)-phosphinic acid chloride

aniline

6-(4-tert.butyl-phenylsulphonylamino)-4-(2-hydroxy-ethoxy)-5-(3-methoxy-phenoxy)-pyrimidine-2-carboxylic acid

→

6-(4-tert.butyl-phenylsulphonylamino)-4-(2-hydroxy-ethoxy)-5-(3-methoxy-phenoxy)-pyrimidine-2-carboxylic acid phenylamide

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter 3 hours the reaction mixture was evaporated
2. 2
   Sonstigepartitioned between ethyl acetate and water
3. 3
   SonstigeThe organic phase was dried
4. 4
   Sonstigeevaporated
5. 5
   Sonstigethe residue purified over silica gel with chloroform

Vorschrift

0.2 ml of Hunig base, 0.052 g of bis-(2-oxo-3-oxazolidinyl)-phosphinic acid chloride and 0.01 ml of aniline were added to a solution of 0.053 g of 6-(4-tert.butyl-phenylsulphonylamino)-4-(2-hydroxy-ethoxy)-5-(3-methoxy-phenoxy)-pyrimidine-2-carboxylic acid in 5 ml of acetonitrile. After 3 hours the reaction mixture was evaporated and partitioned between ethyl acetate and water. The organic phase was dried and evaporated, and the residue purified over silica gel with chloroform. There was obtained 0.032 g of 6-(4-tert.butyl-phenylsulphonylamino)-4-(2-hydroxy-ethoxy)-5-(3-methoxy-phenoxy)-pyrimidine-2-carboxylic acid phenylamide, m.p. 143° C., MS: (M-H)- 591.

Quelle