HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → 5-benzyloxy-N1-methylbenzene-1,2-diamine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | 5-benzyloxy-N-methyl-2-nitroaniline | HCID 67954051 | — |
| Catalyst | HCID 178503042 | HCID 178503042 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | 5-benzyloxy-N1-methylbenzene-1,2-diamine | HCID 67953977 | 94.7% |
Reaction Steps
5% platinum carbon (0.50 g, (DRY)) was added to a 2-propanol (170 mL) suspension of 5-benzyloxy-N-methyl-2-nitroaniline (10.00 g, 38.7 mmol), and catalytic hydrogenation reaction was performed at ordinary pressure. The reaction solution was filtered to remove a catalyst. The catalyst was washed with 2-propanol (20 mL), and the washing liquid was added to the precedent filtrate. Under ice cooling, 97% sulfuric acid (1.06 mL, 19.3 mmol) was added to the mixture, and then the mixture was stirred under the same temperature for 30 minutes. The resulting precipitated crystals were collected by filtration, then washed with 2-propanol (40 mL), and dried at 40° C., thereby obtaining 9.07 g of a light-purple, crystal target compound (yield: 94.7%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08940889B2 |
| Source dataset | uspto-grants-2015_01 |
| ORD ID | ord-c1617e0b284f494d9de7aa602731dd11 |
| Source note | uspto-grants-2015_01 |