HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-(4-Nitro-phenyl)-cyclopropanecarboxylic acid methyl ester → Methyl 1-(4-aminophenyl)cyclopropane-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-(4-Nitro-phenyl)-cyclopropanecarboxylic acid methyl ester | HCID 59129429 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Methyl 1-(4-aminophenyl)cyclopropane-1-carboxylate | HCID 58841079 | 66.1% |
Reaction Steps
To a solution of methyl 1-(4-nitrophenyl)cyclopropanecarboxylate (20 g, 0.09 mol) in MeOH (400 mL) was added Ni (2 g) under nitrogen atmosphere. The mixture was stirred under hydrogen atmosphere (1 atm) at room temperature overnight. The catalyst was filtered off through a pad of Celite and the filtrate was evaporated under vacuum to give crude product, which was purified by chromatography column on silica gel (petroleum ether/ethyl acetate=10:1) to give methyl 1-(4-aminophenyl)cyclopropanecarboxylate (11.38 g, 66%). 1H NMR (300 MHz, CDCl3) δ7.16 (d, J=8.1 Hz, 2H), 6.86 (d, J=7.8 Hz, 2H), 4.31 (br, 2H), 3.61 (s, 3H), 1.55-1.50 (m, 2H), 1.30-1.12 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08598181B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-e79876f672e049568c787ad188458689 |
| Source note | uspto-grants-2013_12 |