HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tert-Butyl hypochlorite → HCID 54582542, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tert-Butyl hypochlorite | HCID 521297 | — |
| Reactant | HCID 21951121 | HCID 21951121 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 54582542 | HCID 54582542 | 75.1% |
Reaction Steps
A solution of 1-(2-hydroxyethyl)-3,3,5,5-tetramethylpiperazin-2-one (125 mg, 0.63 mmol) in methanol (1 ml) was cooled to 0° C. tert-Butylhypochlorite (106 ul, 0.94 mmol) was added. The resulting solution was stirred for 60 minutes, and then concentrated under reduced pressure. The crude material was purified by column chromatography eluting from silica gel with a gradient of 0-8% methanol in dichloromethane to give 111 mg of a white solid. 1H NMR (D2O, 400 MHz) δ 1.21 (s, 3H), 1.43 (s, 3H), 3.36 (s, 2H), 3.43-3.345 (t, J=5.6 Hz, 2H), 3.64-3.66 (t, J=5.6 Hz, 2H). 13C NMR (D2O, 100 MHz) δ 172.9, 68.1, 60.0, 58.4, 57.4, 49.6, 25.5, 22.7. LRMS (ESI/APCI) m/z 235 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09248117B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-ac061659e0a7400893080feea8439cac |
| Source note | uspto-grants-2016_02 |