HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 28384692, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Tert-Butylamine | HCID 6385 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-bromo-4-methoxybenzenesulfonyl chloride | HCID 3863747 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 28384692 | HCID 28384692 | 77% |
Reaction Steps
3-Bromo-4-methoxyphenylsulfonyl chloride (2.80 g, 9.8 mmol) was dissolved in dichloromethane (30 mL) and the solution was treated with triethylamine (1.76 mL, 12.6 mmol), followed by the dropwise addition of t-butylamine (1.33 mL, 12.6 mmol). The mixture was allowed to stand for 2 hours and then was poured onto a mixture of 5% citric acid solution and dichloromethane. The organic layer was separated and the aqueous layer was extracted with dichloromethane (×2). The combined organic layers were dried and concentrated. Crystallization of the crude solid from ethyl acetate/hexane gave 3-bromo-N-tert-butyl-4-methoxybenzenesulfonamide (2.43 g, 77%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08299110B2 |
| Source dataset | uspto-grants-2012_10 |
| ORD ID | ord-f3a26b124faf40858d6c38a7362bd851 |
| Source note | uspto-grants-2012_10 |