HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 19711231, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | HCID 19711229 | HCID 19711229 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 19711231 | HCID 19711231 | 92% |
Reaction Steps
A stirred suspension of methyl 8-amino-7-nitro-1,4-benzodioxan-5-carboxylate (300 mg, 0.0012 mole) in ethanol (30 ml) together with glacial acetic acid (5 ml) was hydrogenareal over 10% Pd-C (100 mg) at atmospheric pressure and temperature for 5 h. The catalyst was filtered off and the filtrate concentrated in vacuo. The residue was basified with concentrated potassium carbonate solution and extracted with ethyl acetate. The extract was dried (Na2SO4) and concentrated in vacuo to afford methyl 7,8-diamino-1,4-benzodioxan-5-carboxylate as a beige solid (240 mg, 92%). 1H NMR (CDCl3) δ:6.91(s,1 H), 4.21(s,4 H), 3.96(br s.2 H), 3.74(s,3 H), 3.0(br s,2 H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05705509 |
| Source dataset | uspto-grants-1998_01 |
| ORD ID | ord-cffc758317bd4280ba76d75e86c2e51f |
| Source note | uspto-grants-1998_01 |