反応 #3540

反応方程式

sodium hydride

2,6-dibromophenylacetonitrile

2,4-diaminopyrimidine-5-carboxaldehyde

→

6-(2,6-dibromo-phenyl)-pyrido[2,3-d]pyrimidine-2,7-diamine

収率 63.3%

溶媒

2-ethoxyethanol

反応条件

後処理

1. 1
   温度The reaction was refluxed for 4 hours
2. 2
   温度cooled
3. 3
   洗浄The residue was washed well with acetonitrile

実験手順

To a solution of 0.23 g 60% sodium hydride suspension in 11.0 mL of 2-ethoxyethanol was added 4.18 g of 2,6-dibromophenylacetonitrile and 2.00 g of 2,4-diaminopyrimidine-5-carboxaldehyde. The reaction was refluxed for 4 hours, cooled, and poured into ice water. The residue was washed well with acetonitrile then diethyl ether to give 3.62 g of 6-(2,6-dibromo-phenyl)-pyrido[2,3-d]pyrimidine-2,7-diamine, CIMS (1% NH3 in CH4): 422=M+ +C2H5, 396 (Base), 394=M+ +H, 393=M+ ; mp 284°-289° C.

出典