HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4-Dimethoxybenzenesulfonyl chloride → 3,4-Dimethoxy-N-[5-(4-methoxyphenyl)-pyrimidine-2-yl]benzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4-Dimethoxybenzenesulfonyl chloride | HCID 2734183 | — |
| Reactant | 5-(4-Methoxyphenyl)pyrimidin-2-amine | HCID 44558590 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | 3,4-Dimethoxy-N-[5-(4-methoxyphenyl)-pyrimidine-2-yl]benzenesulfonamide | HCID 24994813 | 33.2% |
Reaction Steps
To a solution of 5-(4-methoxyphenyl)pyrimidin-2-amine (302 mg, 1.5 mmol) in 10 mL of dry pyridine was added 3,4-dimethoxybenzenesulfonyl chloride (398 mg, 1.68 mmol). The solution was stirred at room temperature under Argon. After 24 h, the pyridine was removed in vacuo and flashed off with toluene. The residue was partitioned between EtOAc and 1M HCl. EtOAc phase was washed with water to neutral, dried over Na2SO4 and evaporated in vacuo to give 0.20 g of a solid which was taken up in 4 mL of hot HOAc, diluted with 2 mL of water which initiated crystallization to give 181 mg of product with mp 218-220° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08071631B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-bdf383b7ed0042f28c7dda1a83ef48cd |
| Source note | uspto-grants-2011_12 |