HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 11371439, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 11471190 | HCID 11471190 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 11371439 | HCID 11371439 | — |
Reaction Steps
A solution of Example 44C (0.40 g, 1.5 mmol) in dichloromethane (9 mL) was treated with pyridine (0.36 mL, 4.4 mmol), treated with methanesulfonyl chloride (0.13 mL, 1.6 mmol), stirred for 4 hours, treated with pyridine (0.2 mL, 2.5 mmol), treated with methanesulfonyl chloride (0.10 mL, 1.3 mmol), stirred for 16 hours,refluxed for 9 hours, cooled to ambient temperature, treated with water (25 mL) and extracted with dichloromethane (3×20 mL). The combined dichloromethane extracts were washed with brine, dried (Na2SO4) and concentrated. Purification of the residue on silica gel with 1:1 ethyl acetate:hexanes provided the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06503935B1 |
| Source dataset | uspto-grants-2003_01 |
| ORD ID | ord-5d2b64c3fbae4fbd970760d9f4eeb4cb |
| Source note | uspto-grants-2003_01 |