تفاعل #4773

معادلة التفاعل

5-(1-hydroxyethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine

phosphorus tribromide

→

5-(1-bromoethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine

المذيبات

tetrahydrofuran

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   استخلاصextracted with ethyl acetate
2. 2
   أخرىThe organic layer was evaporated in vacuo
3. 3
   أخرىThe residue was chromatographed on silicagel
4. 4
   غسيلeluting with chloroform
5. 5
   workup.ADDITIONThe fractions containing the desired product
6. 6
   أخرىevaporated in vacuo
7. 7
   أخرىThe residue was crystallized from diisopropyl ether

الإجراء التجريبي

A solution of 5-(1-hydroxyethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (1.8 g) in tetrahydrofuran (10 ml) was dropped to a solution of phosphorus tribromide (0.34 ml) in tetrahydrofuran (20 ml) under ice cooling. The reaction mixture was stirred for 5 hours at the same condition and poured into ice water and extracted with ethyl acetate. The organic layer was evaporated in vacuo. The residue was chromatographed on silicagel eluting with chloroform. The fractions containing the desired product were combined and evaporated in vacuo. The residue was crystallized from diisopropyl ether to afford 5-(1-bromoethyl)-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (0.3 g).

المصدر