HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 1-(1-Benzyl-4-methylpiperazin-2-yl)methanamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Sodium Sulfate | HCID 24436 | — |
| Reactant | Aluminium lithium hydride | HCID 21226445 | — |
| Reactant | HCID 69206757 | HCID 69206757 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-(1-Benzyl-4-methylpiperazin-2-yl)methanamine | HCID 11775616 | 100% |
Reaction Steps
1M Lithium aluminium hydride in tetrahydrofuran (112 ml, 0.112 mol) was added dropwise to a stirred solution of (RS)-1-benzyl-4-(tert-butyloxycarbonyl)-2-carbamoylpiperazine (D1) (15 g, 0.047 mol) in anhydrous tetrahydrofuran (300 ml) at room temperature under argon. On complete addition the reaction mixture was stirred at room temperature for 0.5 h, then at reflux for a further 1.5 h. The mixture was cooled to room temperature and treated sequentially with water (19.5 ml), 2N sodium hydroxide (22.5 ml) and water (19.5 ml) dropwise. Sodium sulphate was added and the resultant stirred for 0.3 h, filtered and the filtrate evaporated in vacuo to give the title compound (10.3 g, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07365077B2 |
| Source dataset | uspto-grants-2008_04 |
| ORD ID | ord-232abf793bbc4b57b0d5e3745a447d4d |
| Source note | uspto-grants-2008_04 |