HuagongsheHuagongshe Chemistry Print Report · For research reference only
[4-(6-Chloro-5-nitro-pyrimidin-4-ylamino)-phenyl]-acetic acid ethyl ester → [4-(5-Amino-6-chloro-pyrimidin-4-ylamino)-phenyl]acetic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | [4-(6-Chloro-5-nitro-pyrimidin-4-ylamino)-phenyl]-acetic acid ethyl ester | HCID 86625829 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | [4-(5-Amino-6-chloro-pyrimidin-4-ylamino)-phenyl]acetic acid ethyl ester | HCID 86625828 | — |
Reaction Steps
A mixture of [4-(6-chloro-5-nitro-pyrimidin-4-ylamino)-phenyl]-acetic acid ethyl ester (0.400 g, 1.19 mmol) and Raney Ni (˜0.100 g) in THF (10 mL) is stirred for 20.5 h at rt, under a hydrogen atmosphere. The reaction mixture is filtered through a pad of celite and concentrated. Purification of the residue by silica gel column chromatography (Hexane/EtOAc, 70:30) provides the title compound as a yellow solid: ES-MS: 307.1 [M+H]+; single peak at tR=3.81 min (System 1); Rf=0.06 (Hexane/EtOAc, 70:30).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08030311B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-03a9ca05078541318ee63d3fa6e87d65 |
| Source note | uspto-grants-2011_10 |