Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 71743654 | HCID 71743654 | — |
| Catalyst | Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+) | HCID 178418228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 84734218 | HCID 84734218 | 68.7% |
Reaction Steps
A mixture of (2-bromo-5-chlorophenyl)(cyclopropyl)methanamine (2 g, 7.7 mmol), Pd(dppf)Cl2 (0.2 g), DIPEA (3 g, 23.1 mmol) in 20 mL of DMF was heated in an autoclave at 130° C. under 2 MPa of CO (g) for 16 hours. After the reaction, the mixture was diluted with AcOEt (150 mL) and washed with brine (30 mL×3). The organic layer was dried over anhy. Na2SO4, filtered, and concentrated in vacuo to give a crude product which was purified by chromatography to give title compound (1.1 g, yield 68.7%) as a yellow solid. MS: 207.9 (M+H+, 1C1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09133158B2 |
|---|
| Source dataset | uspto-grants-2015_09 |
|---|
| ORD ID | ord-8c7b21be93a04347b293600d6ec73d8c |
|---|
| Source note | uspto-grants-2015_09 |
|---|
