HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 57485783, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 57485781 | HCID 57485781 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 57485783 | HCID 57485783 | 97% |
Reaction Steps
To a solution of 7,9-bis(hydroxymethyl)-1,4-dioxaspiro[4.5]decane (6.3 g, 21 mmol) in dry dichloromethane (100 ml) with triethylamine (8.90 ml, 63.8 mmol) was added methanesulfonyl chloride (4.11 ml, 53.2 mmol) drop-wise at 0° C. The reaction was allowed to come to ambient temperature and stir overnight. The reaction was quenched with saturated sodium bicarbonate (50 ml) and allowed to stir for 15 min. After separation, the aqueous layer was extracted with dichloromethane (1×50 ml). The combined extracts were dried over potassium carbonate, filtered and concentrated to give a dark brown liquid (7.3 g, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07897611B2 |
| Source dataset | uspto-grants-2011_03 |
| ORD ID | ord-8f4eac4382c04852a27255f2c9e49bb5 |
| Source note | uspto-grants-2011_03 |