反応 #3273

反応方程式

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

収率 64.0%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   その他resulting in a clear solution
2. 2
   温度cooled to room temperature
3. 3
   その他The resulting precipitate was removed by filtration
4. 4
   洗浄washed with water
5. 5
   その他The residue was dried
6. 6
   その他purified by flash chromatography
7. 7
   洗浄eluting with a gradient of 1:1 hexane

実験手順

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.

出典