HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13477118, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 13477123 | HCID 13477123 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 13477118 | HCID 13477118 | 49% |
Reaction Steps
To a solution of 3.5 g (0.014 m), of 2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethylamine of Example 6 and 1.4 g (0.014 m) of triethylamine in 50 ml of CH2Cl2, 1.6 g (0.014 m) of methanesulfonyl chloride was added dropwise maintaining the temperature between 15°-20° C. The mixture was stirred 45 minutes, then poured into water. The CH2Cl2 layer was separated, washed with water, dried (Na2SO4), filtered and evaporated to give a foamy solid. Recrystallization from approximately 40 ml of toluene gave 2.27 g (49%) of N-(2-(6,11-dihydro-11-oxodibenz[b,e]oxepin-2-yl)ethyl)methanesulfonamide, m.p. 104°-106° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04526891 |
| Source dataset | uspto-grants-1985_07 |
| ORD ID | ord-4060d379c9a14f408e354972a8697ed6 |
| Source note | uspto-grants-1985_07 |