HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphate → HCID 10172022, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphate | HCID 1061 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | PyBOP | HCID 2724699 | — |
| Reactant | Aminoacetonitrile hydrochloride | HCID 11491918 | — |
| Reactant | N-(2,2,2-Trifluoro-1-phenylethyl)-L-leucine | HCID 57446944 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 10172022 | HCID 10172022 | — |
Reaction Steps
A mixture of N-(2,2,2-trifluoro-1-phenylethyl)-L-leucine (149 mg, 0.50 mmol), aminoacetonitrile hydrochloride (102 mg, 1.1 mmol) and PyBOP (260 mg, 0.50 mmol) was dissolved in DMF (5 mL). Triethylamine (0.3 mL, 2.1 mmol) was added and the mixture was stirred overnight, then poured into pH 3 phosphate buffer and extracted with 3:1 ether/ethyl acetate. The organic phase was washed with saturated aqueous NaHCO3 and brine, dried over MgSO4 and evaporated. Purification by ISCO column chromatography (gradient 20% to 50% ethyl acetate/hexanes) provided N1-(cyanomethyl)-N2-(2,2,2-trifluoro-1-phenylethyl)-L-leucinamide as a 1:1 mixture of diastereomers. MS (+APCI): 313.9 [M+1].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07375134B2 |
| Source dataset | uspto-grants-2008_05 |
| ORD ID | ord-369774ba742d4630ad95f25743832e42 |
| Source note | uspto-grants-2008_05 |