HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → HCID 22958561, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| Reactant | (2S)-1-((tert-butoxy)carbonyl)azetidine-2-carboxylic acid | HCID 2734495 | — |
| Reactant | 6-(Aminomethyl)isoquinolin-1-amine | HCID 22169775 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22958561 | HCID 22958561 | 97.2% |
Reaction Steps
2.00 g 1-Tert.butoxycarbonyl-azetidin-2(S)-carboxylic acid, 1.70 g 1-amino-6-aminomethyl-isoquinolin, 3.50 g TBTU were dissolved in 40 mL DMF. 3.55 mL N-methylmorpholin was added slowly with stirring. The solution was applied to a reversed-phase chromatography column (lenght 100 mm, diameter 14 mm; Merck Lichroprep RP-18, 15-25 u). Elution was started with 25 mL of methanol/water containing 0.3% acetic acid (10 : 90), then a linear gradient to pure methanol over a period of 75 mL was applied followed by 50 mL of pure methanol. Fraktions of 5 mL each were sampled. The solvent was evaporated to give 3.4 g of the tile compound. MS: 357
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06194409B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-3acbb0ca607745cc8c798bad7f4d03f4 |
| Source note | uspto-grants-2001_02 |