HuagongsheHuagongshe Chemistry Print Report · For research reference only
(Diethylamino)sulfur trifluoride → HCID 59726028, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (Diethylamino)sulfur trifluoride | HCID 123472 | — |
| Reactant | HCID 59726021 | HCID 59726021 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59726028 | HCID 59726028 | 54.2% |
Reaction Steps
A mixture of 2-(6-chlorophthalazin-1-yl)propan-2-ol (154 mg, 0.69 mmol) in 5 mL of DCM at −78° C. was treated with DAST (0.11 mL, 0.76 mmol) slowly. It was warmed slowly to room temperature overnight, then quenched with saturated NaHCO3 solution and extracted with CH2Cl2. The DCM layer was dried over MgSO4, filtered and concentrated. Purification on an ISCO (12 g column, 10-35% EtOAc:Hexanes) afforded 6-chloro-1-(2-fluoropropan-2-yl)phthalazine (84 mg, 54% yield) as a pale yellow, viscous oil. MS (ESI, pos. ion) m/z: 225.1 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08101612B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-42cb9035a4da40d7b2d16a315cdff015 |
| Source note | uspto-grants-2012_01 |