HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 11776281, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 3-(Cyclohexyloxy)propan-1-ol | HCID 10034878 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Product | HCID 11776281 | HCID 11776281 | 57.8% |
Reaction Steps
To a solution of 10 parts of 3-(cyclohexyloxy)-1-propanol in 160 parts of dichloromethane there were added 11.2 parts of N,N-diethylethanamine and dropwise 8.14 parts of methanesulfonyl chloride. The whole was stirred for 9 hours at room temperature. The reaction mixture was washed with Na2CO3 (aq.) and water and was then dried, filtered and evaporated. The residue was purified by column chromatography (silica gel; CH2Cl2 /CH3OH 99:1). The eluent of the desired fraction was evaporated and the residue was co-evaporated with methylbenzene. The product was filtered off and dried, yielding 8.6 parts (57.8%) of 3-(cyclohexyloxy)-1-propanol methanesulfonate (ester) (interm. 21).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05262418 |
| Source dataset | uspto-grants-1993_11 |
| ORD ID | ord-56e0b7c361dd4e79bd420a70a1e7502c |
| Source note | uspto-grants-1993_11 |