HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydroxylamine → HCID 178451239, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydroxylamine | HCID 787 | — |
| Reactant | HCID 67529271 | HCID 67529271 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178451239 | HCID 178451239 | 100.1% |
Reaction Steps
To a solution of {tert-butoxycarbonyl-[3-cyanobenzyl]-amino}-acetic acid tert-butyl ester (3.5 g, 0.010 mol) in Ethanol (100 mL) under N2, was added hydroxylamine (1.66 mL, 0.0505 mol) in one portion. After being stirred at RT for 12 h, the reaction mixture was concentrated under reduced pressure to afford the title compound as a pale yellow viscous liquid (3.8 g, 99%). 1H NMR (DMSO-d6, 400 MHz) δ 9.59 (s, 1H), 7.53-7.56 (m, 2H), 7.29-7.33 (m, 1H), 7.24-7.26 (m, 1H), 5.76 (s, 2H), 4.37-4.39 (s, 2H), 3.74 (s, 2H), 1.35-1.37 (s, 18H). LC/MS (Method A): 380.0 (M+H)+. HPLC (Method B) Rt 5.91 min (Purity: 90.3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08202865B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-32d10d9267b44743bf1f625f7644052b |
| Source note | uspto-grants-2012_06 |