HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tert-Butyl hypochlorite → HCID 54581543, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tert-Butyl hypochlorite | HCID 521297 | — |
| Reactant | 1-(2-Hydroxyethyl)-3,3-dimethylpiperazine-2,5-dione | HCID 19958090 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 54581543 | HCID 54581543 | 80% |
Reaction Steps
A solution of 1-(2-hydroxyethyl)-3,3-dimethylpiperazine-2,5-dione (300 mg, 1.61 mmol) in methanol (3 ml) was cooled to 0° C. tert-Butylhypochlorite (272 ul, 2.4 mmol) was added. The resulting solution was stirred for 35 minutes, and then concentrated under reduced pressure. The crude material was purified by column chromatography, eluting the desired product from silica gel with a gradient of 1 to 10% methanol in dichloromethane to give the title compound as a white solid (284 mg, 1.28 mmol, 80%). 1H NMR (D2O, 400 MHz) δ 1.67 (s, 6H), 2.26-2.28 (t, J=5.0 Hz, 1H), 3.59-3.62 (t, J=5.0 Hz, 2H), 3.86-3.90 (q, J=5.0 Hz, 2H), 4.32 (s, 2H); LRMS (ESI/APCI) m/z 221 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09248117B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-7ee8ce1708d74fffb4eec9a90e98091a |
| Source note | uspto-grants-2016_02 |