HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 22185472, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 22185475 | HCID 22185475 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Sodium Bicarbonate | HCID 516892 | — |
| Product | HCID 22185472 | HCID 22185472 | 13% |
Reaction Steps
A solution of methanesulfonyl chloride (33 mg, 0.3 mmol) in dichloromethane (4 ml) was treated with a solution of Example 3 (103 mg, 0.3 mmol) in methanol (1 ml). The mixture was stirred at room temperature for 2 hours then diluted with dichloromethane and sodium hydrogen carbonate solution. The aqueous layer was then separated and extracted with additional dichloromethane. The combined organic layers were then washed with brine, dried over anhydrous magnesium sulphate, filtered and concentrated at reduced pressure. The residue was chromatographed on silica gel eluting with dichloromethane/methanol/0.880 ammonia solution (10:1:0.1) to give the title compound (16 mg, 13%) as a pale yellow solid; MS(ES+) m/e 421/423 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07026336B1 |
| Source dataset | uspto-grants-2006_04 |
| ORD ID | ord-efb5287d556c41b5bd508c28cf051c9b |
| Source note | uspto-grants-2006_04 |