HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyclopropylamine → HCID 24890787, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyclopropylamine | HCID 69828 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | (R)-7-chloro-5-cyclopentyl-4-ethyl-4,5-dihydro-[1,2,4]triazolo[4,3-f]pteridine | HCID 59389586 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 24890787 | HCID 24890787 | — |
Reaction Steps
(R)-7-chloro-5-cyclopentyl-4-ethyl-4,5-dihydro-[1,2,4]triazolo[4,3-f]pteridine (70 mg, 0.23 mmol), cyclopropylamine (0.5 ml, 7.18 mmol), DIPEA (0.16 ml, 0.918 mmol) in nBuOH (2 ml) were heated in a sealed tube in the microwave at 140° C. for 90 minutes. The reaction mixture was concentrated in vacuo, and 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] to afford the title compound as an off-white powder. The free base was generated using a bicarbonate resin, and was freeze-dried to give the title compound as a colourless solid (25.6 mg, 34% yield)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08524902B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-4b4f0523eba446ab9978c9c050374f71 |
| Source note | uspto-grants-2013_09 |