HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 33788030, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | O-Phenylenediamine | HCID 7243 | — |
| Reactant | Cyclopropanecarboxaldehyde | HCID 123114 | — |
| Reactant | Sodium cyanoborohydride | HCID 5003444 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 33788030 | HCID 33788030 | 34.4% |
Reaction Steps
To a solution of benzene-1,2-diamine (1.62 g, 15.0 mmol) and cyclopropanecarbaldehyde (1.05 g, 15.0 mmol) in MeOH (15 mL) at 0° C. was added NaCNBH3 (2.07 g, 33.0 mmol) and acetic acid (0.2 mL). The ice bath was removed and the resulting mixture was stirred at room temperature over night. The resulting mixture was diluted with EtOAc, washed with H2O, dried over Na2SO4, filtered, and concentrated in vacuo. The resultant residue was purified by flash column chromatography (SiO2), eluting with a hexanes-EtOAc gradient to yield N-cyclopropylmethyl-benzene-1,2-diamine (836 mg, 34%). MS 163 (M+1)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08981113B2 |
| Source dataset | uspto-grants-2015_03 |
| ORD ID | ord-06a5a88b0e0f4d899f8f26935d5846ac |
| Source note | uspto-grants-2015_03 |