HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 23121900, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 69645660 | HCID 69645660 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 23121900 | HCID 23121900 | 88% |
Reaction Steps
Bis(1,1-dimethylethyl)2-(hydroxymethyl)-2-(phenylmethyl)piperazine-1,4-dicarboxylate (3.6 g, 8.9 mmol) was dissolved in N,N-dimethylformamide (40 mL). 60% Sodium hydride (0.43 g, 11 mmol) was added thereto, and the mixture was stirred at room temperature for 3 hours. To the reaction solution was added a 0.5 M aqueous sodium hydrogen carbonate solution, and the resulting mixture was extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. To the residue was added diethyl ether, and the precipitated crystals were collected by filtration to obtain the title compound (2.6 g, yield 88%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07795267B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-b45dc414ea564d77806b8014ba762f7b |
| Source note | uspto-grants-2010_09 |