HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 4-[6-chloro-4-(3-methanesulfonyl-benzenesulfonyl)-3,4-dihydro-2H-benzo[1,4]oxazin-8-yl]-piperazine-1-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 3-(Methylsulfonyl)benzenesulfonyl chloride | HCID 220330 | — |
| Reactant | 4-(6-chloro-3,4-dihydro-2H-benzo[1,4]oxazin-8-yl)-piperazine-1-carboxylic acid tert-butyl ester | HCID 20765688 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-[6-chloro-4-(3-methanesulfonyl-benzenesulfonyl)-3,4-dihydro-2H-benzo[1,4]oxazin-8-yl]-piperazine-1-carboxylic acid tert-butyl ester | HCID 69066439 | 92% |
Reaction Steps
3-Methanesulfonyl-benzenesulfonyl chloride (80 mg, 0.314 mmol) was added in small portions under nitrogen to an ice-cold solution of 4-(6-chloro-3,4-dihydro-2H-benzo[1,4]oxazin-8-yl)-piperazine-1-carboxylic acid tert-butyl ester (101 mg, 0.285 mmol) and pyridine (50 mg, 0.628 mmol) in dichlormethane (2 mL). After 1.5 hours at ambient temperature, water was added. The layers were separated and the organic phase was washed with saturated aqueous solution of sodium bicarbonate (20 mL), dried (Na2SO4) and concentrated to give 4-[6-chloro-4-(3-methanesulfonyl-benzenesulfonyl)-3,4-dihydro-2H-benzo[1,4]oxazin-8-yl]-piperazine-1-carboxylic acid tert-butyl ester as an oil (150 mg, 91%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08377931B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-3c6056dbc33249ffbb9c450021d2a47a |
| Source note | uspto-grants-2013_02 |