HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 22632190, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-Methylthio-2-imidazoline hydroiodide | HCID 88369 | — |
| Reactant | HCID 54417205 | HCID 54417205 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 22632190 | HCID 22632190 | 61.8% |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A mixture of methyl (±)-8-[3-amino-1-propyloxy]-2-methyl-3-oxo-2,3,4,5-tetrahydro-1H-2-benzazepine-4-acetate (0.3 g, 1 mmol), 2-methylthioimidazoline (0.46 g, 2 mmol), diisopropylethylamine (0.42 mL, 2 mmol) and dimethylacetamide (3 mL) was heated to 100° C. under argon. After 2 hr, the reaction was concentrated under vacuum and the residue was partitioned between CHCl3 and H2O. The organic phase was dried (MgSO4) and concentrated, and the residue was purified by preparative HPLC to give the title compound (0.24 g, 51%) as a yellow oil: MS (ES) m/e 389.4 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06825188B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-4a34a1314f0b445ea2289f7e7f7ac9e4 |
| Source note | uspto-grants-2004_11 |