HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,4,6-Trimethylpyridine → HCID 67981371, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,4,6-Trimethylpyridine | HCID 7953 | — |
| Reactant | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Reactant | Trifluoroacetic acid--1-(2-aminoethyl)-1H-pyrrole-2,5-dione (1/1) | HCID 16212752 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 67981371 | HCID 67981371 | — |
Reaction Steps
N-(2-Aminoethyl)maleimide TFA salt (51 mg, 0.20 mmol) and Eei-AOAc-OSu (77 mg, 0.30 mmol) were dissolved in NMP (2 mL). Sym.-collidine (80 μL, 0.6 mmol) was added and the reaction mixture stiffed for 70 min. The reaction mixture was diluted with water (7 mL) and the product, eei-aminooxyacetyl-maleimide, purified by semi-preparative HPLC. Purification using semi-preparative HPLC (gradient: 15-30% B over 40 min where A=water/0.1% acetic acid and B=ACN) affording 43 mg (75%) pure Eei-aminooxyacetyl-maleimide. The purified material, eei-aminooxyacetyl-maleimide, was characterised by LC-MS (gradient: 10-40% B over 5): tR: 1.93 min. found m/z: 284.1, expected MH+: 284.1
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09061080B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-b508657652f948408de7561a63840afb |
| Source note | uspto-grants-2015_06 |