반응 #3540

반응 방정식

sodium hydride

2,6-dibromophenylacetonitrile

2,4-diaminopyrimidine-5-carboxaldehyde

→

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

수율 63.3%

용매

2-ethoxyethanol

반응 조건

후처리

1. 1
   온도The reaction was refluxed for 4 hours
2. 2
   온도cooled
3. 3
   세척The residue was washed well with acetonitrile

실험 절차

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.

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