HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → N-[(2S)-2-(tert-butoxycarbonylamino)-3-(phenylmethoxy)propyl]-N-[2-(tert-butoxycarbonylamino)-3-(phenylmethoxy)Propyl]amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | (S)-tert-butyl 3-(benzyloxy)-1-oxopropan-2-ylcarbamate | HCID 11196731 | — |
| Reactant | N2-Boc-(S)-3-(benzyloxy)propane-1,2-diamine | HCID 60204732 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | N-[(2S)-2-(tert-butoxycarbonylamino)-3-(phenylmethoxy)propyl]-N-[2-(tert-butoxycarbonylamino)-3-(phenylmethoxy)Propyl]amine | HCID 66639988 | 22.1% |
Reaction Steps
The product from Example 17B (0.35 g, 1.25 mmol) and the product from Example 17A (0.36 g, 1.29 mmol) in absolute ethanol (12 mL) were treated with sodium cyanoborohydride (94 mg, 1.50 mmol) and a catalytic amount of acetic acid. The resulting mixture was stirred at ambient temperature overnight. The mixture was partitioned between water (40 mL) and ethyl acetate (3×40 mL). The organic layers were combined, dried over Na2SO4, filtered, and concentrated under reduced pressure. The residue was subjected to column chromatography on silica gel (hexanes:ethyl acetate, 1:1) to provide the title compound (0.15 g, 22%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08524753B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-5f4d3eb232c64b089e19cd6883476933 |
| Source note | uspto-grants-2013_09 |