HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 131731932, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Cyclopropylamine | HCID 69828 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Reactant | HCID 86621492 | HCID 86621492 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 131731932 | HCID 131731932 | 68.8% |
Reaction Steps
The product from Example 250, Part 4 (174 mg, 0.644 mmol) and cyclopropylamine (35.6 mg, 0.611 mmol) were dissolved in methanol (6.0 mL). That solution was treated with acetic acid (0.209 mL) and sodium cyanoborohydride (38.4 mg, 0.611 mmol). The reaction mixture was stirred at rt overnight. It was concentrated, diluted with ethyl acetate and washed with a saturated NaHCO3 solution. The organic layer was dried over MgSO4, filtered and concentrated. The residue was flash chromatographed (silica, 5% to 6% to 10% MeOH/CH2Cl2) to provide the desired product as a colorless oil (131 mg, 68.8% yield). LCMS: m/z 312.2 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08853243B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-c297d1b903e24c4fac1b6023742c2cd6 |
| Source note | uspto-grants-2014_10 |