HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 57961752, compound → HCID 57961539, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 57961752 | HCID 57961752 | — |
| Catalyst | Iron | HCID 23925 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 57961539 | HCID 57961539 | 87.3% |
Reaction Steps
To a solution of tert-butyl {3-[(3-nitrobenzoyl)amino]phenyl}carbamate (2.00 g, 5.6 mmol) in water (4 mL), methanol (22 mL) and acetic acid (8.6 mL) was added iron (0.782 g, 14.0 mmol) powder in small quantities. When the addition was completed, the mixture was stirred in water bath for 3 h. The mixture was filtered, and the cake was washed with MeOH/EtOAc. The brown filtrate was concentrated and diluted with H2O, and the aqueous layer was extracted with EtOAc three times. The combined organic layers were dried, filtered and concentrated to give the desired product as an off-white powder (1.6 g, 87%). LCMS for C18H21N3O3 (M+H)+: m/z=328.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08871753B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-ebd1b5801f7f4f75b1f40557ea655cba |
| Source note | uspto-grants-2014_10 |