HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 53743045, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Tetrahydropyran-2-methanol | HCID 7524 | — |
| Reactant | Chlorosulfamic acid | HCID 24499 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Product | HCID 53743045 | HCID 53743045 | — |
Reaction Steps
To a cold solution (-5° C.) of tetrahydropyran-2-methanol (2.33 g, 0.02 mol) in DMF (40 ml) was added 50% oily sodium hydride (1.17 g, 0.024 mol as NaH). After stirring for 45 min, sulfamoyl chloride (3.42 g, 0.03 mol) was added and the stirring continued for an additional 45 min, at -5° C. The reaction mixture was poured into cold water and extracted with chloroform. The organic layer was dried (Na2SO4) and the solvents were removed under vacuum to give a syrup which was dry column chromatographed (eluted with ethyl acetate:hexane, 4:1 v/v) to give pure (tetrahydro-2H-pyran-2-yl) methanesulfamate as a pale yellow syrup, IR:(CHCl3) 1180 cm-1 and 1370 cm-1 (OSO2NH2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04513006 |
| Source dataset | uspto-grants-1985_04 |
| ORD ID | ord-51585397f8274e43b5b05ab6d6a07d57 |
| Source note | uspto-grants-1985_04 |