HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 14013854, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | N-Methylcyclopropanamine | HCID 11029756 | — |
| Reactant | HCID 14013848 | HCID 14013848 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 14013854 | HCID 14013854 | 15.5% |
Reaction Steps
To a mixture of 6.0 g (0.017 mol) of product from Example 105, 1.71 g (0.017 mol) of triethylamine in 30 ml of DMF was added 1.76 g (0.025 mol) of N-methylcyclopropylamine at such a rate that the temperature remained below 30° C. After 4 hours the reaction mixture was poured into 3.7% HCl and extracted with diethyl ether. The ether phase was washed with H2O, and dried (MgSO4). The dry ether phase was concentrated in vacuo to 5.8 g of a green oil. The crude product was purified by HPLC in 5% ethyl acetate/cyclohexane, followed by kugelrohr distillation at 67 Pa, oven temperature 150° C., affording 1.02 g (15.5%) of product as a green oil, nD25 1.4758.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04921530 |
| Source dataset | uspto-grants-1990_05 |
| ORD ID | ord-5a5d4409f8e047e78b2f2f7d0ce6c3e4 |
| Source note | uspto-grants-1990_05 |