HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 12237610, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 3,6-Dichloropyridazine | HCID 67331 | — |
| Reactant | 3-(Dimethylamino)-1-propanol | HCID 76646 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 12237610 | HCID 12237610 | — |
Reaction Steps
To a solution of 3-dimethylamino-propanol (95 μL) in 5 mL of THF at 0° C. was added NaH (20 mg). The mixture was stirred for 5 min; then 3,6-dichloropyridazine (100 mg) was added and the mixture was allowed to warm to room temperature and stirred overnight at this temperature. The mixture was diluted with 5 mL of water and 5 mL of EtOAc, the phases were separated, and the aqueous phase was extracted with 2×5 mL of EtOAc. The combined organics were washed with 5 mL of brine, dried over Na2SO4 and concentrated to a colorless oil (128 mg) that was used without further purification. Mass spectrum (ESI) 215.9 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06498165B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-cbb1245c24fe49a5adb595af7534355a |
| Source note | uspto-grants-2002_12 |