반응 #67622

반응 방정식

carbonate

(R)-7-chloro-5-cyclopentyl-4-ethyl-4,5-dihydro-[1,2,4]triazolo[4,3-f]pteridine

methylamine

TFA

→

title compound

수율 61.0%

(R)-5-cyclopentyl-4-ethyl-N-methyl-4,5-dihydro-[1,2,4]triazolo[4,3-f]pteridin-7-amine

수율 61.0%

용매

acetonitrile water

ethanol

반응 조건

후처리

1. 1
   기타was sealed
2. 2
   온도After cooling
3. 3
   기타the solvent was removed under reduced pressure
4. 4
   기타the crude product was purified by reverse phase preparative HPLC [Waters Sunfire C18, 10 M, 100 Å column, gradient 10%-95% B (solvent A: 0.05% TFA in water; solvent B: CH3CN) over 16 minutes at 25 mL/min]
5. 5
   기타The free base was obtained

실험 절차

In a vial containing (R)-7-chloro-5-cyclopentyl-4-ethyl-4,5-dihydro-[1,2,4]triazolo[4,3-f]pteridine (70 mg, 0.23 mmol) was added a solution of methylamine in ethanol (2 mL, 2M soln.) The vessel was sealed then heated at 50° C. for 18 hours. After cooling, the solvent was removed under reduced pressure and the crude product was purified by reverse phase preparative HPLC [Waters Sunfire C18, 10 M, 100 Å column, gradient 10%-95% B (solvent A: 0.05% TFA in water; solvent B: CH3CN) over 16 minutes at 25 mL/min]. The free base was obtained by passing the TFA salt in acetonitrile/water through a carbonate cartridge to afford the title compound as a white powder (42 mg, 61% yield).

출처