تفاعل #88897

معادلة التفاعل

2-(4-methoxycarbonylpyrazol-1-yl)adenosine

methylamine

→

2-[4-[(methylamino)carbonyl]-1H-pyrazol-1-yl]adenosine

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   workup.WAITThe produced solution is left
2. 2
   workup.WAITto stand at the given temperature for additional 15 hours
3. 3
   ترشيحThe solution is then filtered with active charcoal
4. 4
   تركيزthe filtrate is concentrated in vacuo
5. 5
   workup.DISSOLUTIONis dissolved in 2 ml of dimethylsulfoxide
6. 6
   workup.WAITleft
7. 7
   درجة الحرارةto cool down freely to room temperature
8. 8
   workup.ADDITIONThe resulting turbid solution is added to 20 ml of methanol
9. 9
   workup.STIRRINGThe separated gel-like precipitate is stirred under the boil for 1.5-2.5 hours
10. 10
    أخرىwherein a powder-like suspension is formed
11. 11
    درجة الحرارةAfter cooling down
12. 12
    أخرىdrying

الإجراء التجريبي

A suspension of 1 g of 2-(4-methoxycarbonylpyrazol-1-yl)adenosine in 10 ml of 40% methylamine in methanol is stirred in a closed flask at 20° C. until formation of a solution (3 to 5 hours). The produced solution is left to stand at the given temperature for additional 15 hours. The solution is then filtered with active charcoal and the filtrate is concentrated in vacuo. The evaporation residue, which is the amorphous form of 2-[4-[(methylamino)carbonyl]-1H-pyrazol-1-yl]adenosine, is dissolved in 2 ml of dimethylsulfoxide and left to cool down freely to room temperature. The resulting turbid solution is added to 20 ml of methanol. The separated gel-like precipitate is stirred under the boil for 1.5-2.5 hours, wherein a powder-like suspension is formed. After cooling down, sucking off, and drying, 0.8 g of 2-[4-[(methylamino)carbonyl]-1H-pyrazol-1-yl]adenosine polymorph E is obtained.

المصدر