HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 68454854, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 4-Hydroxypyrrolidine | HCID 98210 | — |
| Reactant | 6-Bromo-1-chlorophthalazine | HCID 22030424 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68454854 | HCID 68454854 | — |
Reaction Conditions
| Temperature | 180 °C |
|---|
Reaction Steps
The mixture of 6-bromo-1-chlorophthalazine (Example 1, 0.12 g, 0.5 mmol), pyrrolidin-3-ol (0.08 mL, 1.0 mmol) and potassium carbonate (0.07 g, 0.5 mmol) in 5 mL acetonitrile was added to a glass microwave reaction vessel. The reaction mixture was stirred and heated in a Smith Synthesizer® microwave reactor (Personal Chemistry, Inc., Upssala, Sweden) at 180° C. for 20 min. After about 20 min., all starting material was converted to product (M+1=294, 296). The mixture was concentrated under vacuum and purified via flash chromatography (silica gel) eluting with a gradient of 2% 2 M ammonia in MeOH/DCM to 6% 2M ammonia in MeOH/DCM to give 0.13 1-(6-bromophthalazin-1-yl)pyrrolidin-3-ol as yellow solid. Found MS (ES+): 294, 296(M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07759337B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-0053d213089a4beca5721c0633a6b98d |
| Source note | uspto-grants-2010_07 |