تفاعل #496004

معادلة التفاعل

sodium hydride

8-(2-chlorophenyl)-6-(4-ethylpiperazin-1-yl)-2-methyl-9H-purine

bromomethyl methyl ether

→

title compound

المردود 11.1%

8-(2-Chlorophenyl)-6-(4-ethylpiperazin-1-yl)-9-(methoxymethyl)-2-methyl-purine

المردود 11.1%

المذيبات

tetrahydrofuran

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةWarm the reaction mixture to room temperature
2. 2
   workup.STIRRINGstir for one hour
3. 3
   أخرىQuench the reaction mixture with water
4. 4
   أخرىremove the tetrahydrofuran
5. 5
   أخرىby evaporation
6. 6
   استخلاصextract the reaction mixture with dichloromethane
7. 7
   تجفيفDry the organic layer over anhydrous sodium sulfate
8. 8
   ترشيحfilter
9. 9
   تركيزconcentrate
10. 10
    أخرىto give the residue
11. 11
    أخرىPurify the residue through preparative reverse phase HPLC (X-Bridge column, 5 mM NH4OAc/acetonitrile)

الإجراء التجريبي

Add sodium hydride (0.031 g, 0.0013 mol) to a solution of 8-(2-chlorophenyl)-6-(4-ethylpiperazin-1-yl)-2-methyl-9H-purine (0.233 g, 0.00065 mol) in dry tetrahydrofuran (20 mL) at 0° C. Stir the reaction mixture for 15 min, then cool to −30° C. and add bromomethyl methyl ether (0.081 g, 0.00065 mol). Warm the reaction mixture to room temperature and stir for one hour. Quench the reaction mixture with water, remove the tetrahydrofuran by evaporation and then extract the reaction mixture with dichloromethane. Dry the organic layer over anhydrous sodium sulfate, filter, and concentrate to give the residue. Purify the residue through preparative reverse phase HPLC (X-Bridge column, 5 mM NH4OAc/acetonitrile) to give the title compound (0.029 g). ES/MS m/z 401 (M+1).

المصدر