HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 69356882, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 3-Chloropropanesulphonyl chloride | HCID 15410 | — |
| Reactant | HCID 67512486 | HCID 67512486 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 69356882 | HCID 69356882 | 99.5% |
Reaction Steps
To a solution of 5-amino-isophthalic acid 1-tert-butyl ester 3-methyl ester (D79) (5.0 g, 20 mmol, 1 equiv), DMAP (0.3 g, 2.46 mmol, 0.12 equiv) and pyridine (1.64 g, 20 mmol, 1 equiv) in CH2Cl2 (80 ml) was added 3-chloropropanesulfonyl chloride (2.4 ml, 20 mmol, 1 equiv) dropwise. The resulting mixture was stirred for 16 h then diluted with AcOEt (150 ml). The organic phase was washed with 2N aqueous HCl solution and saturated aqueous NaHCO3 solution, dried over MgSO4 and concentrated in vacuo to give 5-(3-chloro-propane-1-sulfonylamino)-isophthalic acid 1-tert-butyl ester 3-methyl ester (D81) (7.8 g, 99%) as a pale orange solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07253198B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-c00cfb4c4deb4bb2b236983ebabc4de1 |
| Source note | uspto-grants-2007_08 |