HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Acetate → 4-Fluoro-5-methoxy-2-methyl-1H-indole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | 1-(2-Fluoro-3-methoxy-6-nitrophenyl)propan-2-one | HCID 22030743 | — |
| Catalyst | titanium(III) trichloride | HCID 10313229 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | 4-Fluoro-5-methoxy-2-methyl-1H-indole | HCID 22030728 | 91% |
Reaction Steps
To a solution of 3-acetylmethyl-2-fluoro-1-methoxy-4-nitrobenzene (11.36 g, 50 mmol) in acetone (200 ml) was added 4M aqueous ammonium acetate (700 ml) followed by a solution of titanium trichloride (15% in water, 340 ml) dropwise. The mixture was stirred for 10 minutes at ambient temperature and the mixture was extracted with ether. The organic layer was washed with 0.5N aqueous sodium hydroxide followed by water, brine, dried (MgSO4) and the volatiles were removed under vacuum. The residue was purified by column chromatography eluting with methylene chloride to give 4-fluoro-5-methoxy-2-methylindole (8.15 g, 90%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08293902B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-d1df178efc304e6fa9a86b743dc2f90f |
| Source note | uspto-grants-2012_10 |