HuagongsheHuagongshe Chemistry Print Report · For research reference only
DL-valine → Tert-butyl 2-amino-3-methylbutanoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | DL-valine | HCID 1182 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | tert-Butyl acetate | HCID 10908 | — |
| Product | Tert-butyl 2-amino-3-methylbutanoate | HCID 4532027 | — |
Reaction Steps
To a stirred solution of DL-valine (25 g, 0.213 mol) in tert-butyl acetate (250 mL) at 00° C., was added HClO4 (64.2 g, 0.320 mol) portionwise. The reaction mixture was stirred for 36 h at RT. It was diluted with water and extracted in ethyl acetate (500 mL). The organic layer was washed with a 10% sodium bicarbonate solution (2×150 mL), dried over Na2SO4 and concentrated, affording of the title compound as brown liquid. 1H NMR (DMSO-d6, 400 MHz) δ 7.31 (brs, 2H), 3.62 (d, J=4.4 Hz, 1H), 1.98 (d, J=1.7 Hz, 1H), 1.44 (s, 9H), 0.95 (m, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029405B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-c394bcdcf3414ee8b470c0b7e3dfa761 |
| Source note | uspto-grants-2015_05 |