HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 11022760, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 4-Fluorobenzaldehyde | HCID 68023 | — |
| Reactant | HCID 12649914 | HCID 12649914 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 11022760 | HCID 11022760 | 55.4% |
Reaction Steps
##STR29## To a stirred solution of 4-hydroxymethyl-2-methyl-1(2H)-pthalazinone (350 mg, 1.84 mmol) (prepared according to the procedure described in Chem. Pharm. Bull., 28 (1980) 2763) in dry DMF (30 mL) was added NaH (88 mg, 3.68 mmol) in portions over 30 min at 25-30° C., followed by 4-fluorobenzaldehyde (228 mg, 1.84 mmol) added dropwise, keeping the temperature between 0-15° C. The reaction mixture was stirred at room temperature further for 6 h. Ice (200 g) was added to the reaction mixture and extracted with EtOAc. The EtOAc layer was washed with water, dried over anhydrous Na2SO4 and concentrated to obtain the title compound (300 mg, 50%). mp: 168-170° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06011036 |
| Source dataset | uspto-grants-2000_01 |
| ORD ID | ord-27cbf003b4264595b83cba1096c10187 |
| Source note | uspto-grants-2000_01 |