HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 51111672, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,6-Difluorobenzonitrile | HCID 74695 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 51111672 | HCID 51111672 | 75.4% |
Reaction Steps
In a round bottom flask, sodium hydride (60%) (2.40 g; 60 mmol) was suspended in DMF (25 mL) and cooled in an ice water bath under nitrogen. 1-Boc-piperazine (9.53 g; 50.6 mmol) was added in small portions to the reaction mixture at 0° C. over 30 minutes. The mixture was allowed to stir at room temperature for 3 hours and the recooled to 0° C. 2,6-Difluorobenzonitrile (8.57 g; 60 mmol) was added to the reaction mixture in DMF (10 mL) over 45 minutes. The mixture was stirred at room temperature for 16 hours. The reaction mixture was poured in ice water (250 mL) and stirred. The solid was collected by vacuum filtration and washed with water. And then dried under vacuum to yield the title compound (11.65 g; 75% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07985755B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-263f134ed7c748a19aaf1457b2fa19b8 |
| Source note | uspto-grants-2011_07 |