Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | Methyl 1-cyanocyclobutane-1-carboxylate | HCID 25918826 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58193743 | HCID 58193743 | 60.6% |
Reaction Steps
8.74 g (0.063 mol) of 4 and 50 mL of methanol were mixed, after which the mixture was added dropwisely into 3.77 g (4.25 mL) of ethylene diamine to form a reaction solution. The reaction solution was subjected to reaction at room temperature for 15 hours, followed by evaporation to obtain yellow oil. The yellow oil was stirred with water and was mixed with HCl to adjust pH to 2 to obtain a crude product. The crude product was purified by placing in a column (3×20 cm) filled with 100 mL of AG 50 W×8 cationic exchange resin and elutriating with water and HCl solution having gradient concentrations, collecting an eluent fraction of a gradient concentration from 0.5 N to 1.0 N, and followed by evaporating the eluent fraction to obtain 6.37 g (0.038 mol, 60.49%) of 5.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08354512B2 |
|---|
| Source dataset | uspto-grants-2013_01 |
|---|
| ORD ID | ord-8f239b632c104893b0d01703d0e69635 |
|---|
| Source note | uspto-grants-2013_01 |
|---|