HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Ethanediamine, N1,N1,N2-trimethyl- → HCID 86687243, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Ethanediamine, N1,N1,N2-trimethyl- | HCID 67338 | — |
| Reactant | HCID 86687242 | HCID 86687242 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 86687243 | HCID 86687243 | 98.6% |
Reaction Steps
A solution of Intermediate 140a (250 mg, 0.99 mmol) and N,N,N′-trimethylethylenediamine (0.32 mL, 2.48 mmol) in IPA (2.5 mL) was heated to 120° C. for 10 mins under microwave irradiation. The cooled reaction mixture was concentrated in vacuo and the residue was partitioned between EtOAc and water. The phases were separated and the aqueous layer was extracted with EtOAc (×2). The combined organic phase was washed with brine, dried (Na2SO4) and concentrated in vacuo to give the title compound (0.31 g, quant.) as a golden oil that was used in the next step without purification. LCMS (Method 3): Rt 2.51 min, m/z 318.3 [MH+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09145413B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-f6ce6e1bbed14305b42be1d321b7ac30 |
| Source note | uspto-grants-2015_09 |