HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → Methyl 3-bromomethyl-2-chloro-4-methylsulfonylbenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Benzoyl Peroxide | HCID 7187 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Methyl 2-chloro-3-methyl-4-methylsulfonylbenzoate | HCID 15132838 | — |
| Solvent | Carbon Tetrachloride | HCID 5943 | — |
| Product | Methyl 3-bromomethyl-2-chloro-4-methylsulfonylbenzoate | HCID 10969914 | 83.9% |
Reaction Steps
12.1 g of methyl 2-chloro-4-methanesulfonyl-3-methylbenzoate was dissolved in 250 ml of carbon tetrachloride, and the solution was refluxed under stirring. Then, 7.5 g of bromine and 1 g of benzoyl peroxide were gradually added thereto over a period of 30 minutes, and the solution was further refluxed for 4 hours under heating. After cooling, 200 ml of chloroform was added thereto, and the mixture was washed with a 5% sodium hydrogensulfite aqueous solution. The organic layer was separated and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain a crude product. The crude product was washed with ethyl ether to obtain 13.2 g of crystals of the desired product. Melting point: 77°-78° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04885022 |
| Source dataset | uspto-grants-1989_12 |
| ORD ID | ord-eea9891912014136bbfac152d970906f |
| Source note | uspto-grants-1989_12 |