HuagongsheHuagongshe Chemistry Print Report · For research reference only
Oxalyl chloride → HCID 23502546, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | HCID 23502623 | HCID 23502623 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 23502546 | HCID 23502546 | 68.2% |
Reaction Steps
To a solution of 2-{2-chloro-4-methylsulfonyl-3-{[(1-methyl-1Htetrazol-5-yl)thio]-methyl}benzoyl}cyclohexane-1,3-dione (1.0 g) in dichloromethane (100 ml), oxalyl chloride (0.91 g) and 2 drops of N,N-dimethylformamide were added dropwise and the mixture was refluxed for 3 hours. The residue obtained by distilling off the solvent after the reaction was purified by silica gel column chromatography (eluant:ethyl acetate:hexane=7:3) to obtain the objective 3-chloro2-{2-chloro-4-methylsulfonyl-3-{[(1-methyl-1H-tetrazol-5-yl)thio]methyl}benzoyl}-2-cyclohexen-1-one (0.71 g). IR (NaCl):=1662,1310,1279, 1150 cm−1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06770599B2 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-7335788ef4bc4f20a483c7a4ff785875 |
| Source note | uspto-grants-2004_08 |