HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 6-Bromo-1-(3-methoxypropyl)-3-methyl-1H-indazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ammonium Acetate | HCID 517165 | — |
| Reactant | (3-Methoxypropyl)hydrazine | HCID 20516966 | — |
| Reactant | Methanesulfonic acid 2-acetyl-5-bromophenyl ester | HCID 86071609 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | 6-Bromo-1-(3-methoxypropyl)-3-methyl-1H-indazole | HCID 23156223 | — |
Reaction Steps
A mixture of 10.90 g methanesulfonic acid 2-acetyl-5-bromo-phenyl ester, 7.75 g of (3-methoxy-propyl)-hydrazine and 7.17 g of ammonium acetate in 100 ml of o-xylene is refluxed for 3 days with continuous separation of the water which is formed during the reaction. The reaction mixture is then cooled to room temperature and concentrated by evaporation. The title compound is obtained as an orange-yellow oil from the residue by means of flash chromatography (SiO2 60F). Rf=0.38 (1:1 EtOAc-heptane). Rt=4.52 (gradient I).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07868036B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-f7b92177327a47ed90865467c01f2ce8 |
| Source note | uspto-grants-2011_01 |