HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 67378212, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 12532948 | HCID 12532948 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 67378212 | HCID 67378212 | 62% |
Reaction Steps
To a solution of (RS)-1-benzyl-4-(2-hydroxymethyl-phenyl)-azepan-4-ol (7.0 g, 22 mmol) and triethylamine (3.1 ml, 22 mmol) in tetrahydrofuran (80 ml) was added a solution of methanesulfonyl chloride (1.7 ml, 22 mmol) in tetrahydrofuran (20 ml) at 0° C. After completed addition the temperature was allowed to rise to room temperature. Stirring for 2 h was followed by addition of another portion of triethylamine (3.1 ml, 22 mmol). Stirring was continued over night. The reaction mixture was partitioned between water and ethyl acetate. The layers were separated and the organic layer was concentrated in vacuo. Flash column chromatography using heptane/ethyl acetate as eluent gave the title compound as a light yellow oil (4.0 g, 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08664216B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-be1f6829356e4c849d6cd0103a557309 |
| Source note | uspto-grants-2014_03 |