反応 #3324

反応方程式

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

NaH

3-bromobenzyl bromide

→

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

収率 58.0%

溶媒

dimethylformamide

反応条件

後処理

1. 1
   その他resulting in a clear solution
2. 2
   その他The heating mantle was removed
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 solid was purified by flash chromatography
6. 6
   洗浄eluting with 1:1 hexane
7. 7
   乾燥ethyl acetate, then dried in vacuo

実験手順

To a suspension of NaH (60% in mineral oil, 38 mg) in 8 mL of dimethylformamide was added 2-amino-6-(2,6-dichlorophenyl)-pyrido[2,3-d]pyrimidin-7(8H)-one (200 mg, 0.65 mmol). The mixture was heated at 50° C. for 20 minutes resulting in a clear solution. The heating mantle was removed, and 3-bromobenzyl bromide (240 μL, 0.96 mmol) was added. After 10 minutes, the reaction mixture was poured onto 30 mL of ice water. The resulting precipitate was removed by filtration and washed with water. The solid was purified by flash chromatography, eluting with 1:1 hexane:ethyl acetate, then dried in vacuo to provide 178 mg (58%) of 2-amino-8-(3-bromobenzyl)-6-(2,6-dichlorophenyl)-8H-pyrido[2,3-d]pyrimidin-7-one; mp softens at 195° C., melts at 215° C.

出典