تفاعل #3273

معادلة التفاعل

2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one

NaH

1-Iodobutane

→

2-amino-8-butyl-6-(2,6-dichlorophenyl)-8H-pyrido[2,3-d]pyrimidin-7-one

المردود 64.0%

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   أخرىresulting in a clear solution
2. 2
   درجة الحرارةcooled to room temperature
3. 3
   أخرىThe resulting precipitate was removed by filtration
4. 4
   غسيلwashed with water
5. 5
   أخرىThe residue was dried
6. 6
   أخرىpurified by flash chromatography
7. 7
   غسيلeluting with a gradient of 1:1 hexane

الإجراء التجريبي

To a suspension of NaH (60% in mineral oil, 34 mg) in 6 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (202 mg, 0.66 mmol). The mixture was heated to 50° C., resulting in a clear solution. 1-Iodobutane (105 μL, 0.92 mmol) was added, and the solution was stirred at 50° C. for 30 minutes, then cooled to room temperature and poured onto 40 mL of ice water. The resulting precipitate was removed by filtration and washed with water. The residue was dried and purified by flash chromatography, eluting with a gradient of 1:1 hexane:ethyl acetate to all ethyl acetate to provide 152 mg (64%) of 2-amino-8-butyl-6-(2,6-dichlorophenyl)-8H-pyrido[2,3-d]pyrimidin-7-one; mp 202°-205° C.

المصدر