HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 9903958, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 15434529 | HCID 15434529 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 9903958 | HCID 9903958 | 74.8% |
Reaction Steps
A solution of 0.81 g (3 mmol) of 3-fluoro-5-(N-ethylsulfonylamino)-6,7,8,9-tetrahydro-5H-benzocyclohepte (Example 1) in 10 ml of DMA was added dropwise under argon to a suspension of 0.12 g (4.1 mmol) of 80 percent sodium hydride in 5 ml of DMA. After stirring at RT for 3 h, 0.63 g (4.5 mmol) of methyliodide was added dropwise and the mixture was stirred overnight at RT. After distilling off the solvent, the residue was treated with water and extracted with EA. The organic phase was concentrated in vacuo after drying over sodium sulfate. 0.64 g of 3-fluoro-5-(N-ethylsulfonyl-N-methylamino)-6,7,8,9-tetrahydro-5H-benzocycloheptene was obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06908947B2 |
| Source dataset | uspto-grants-2005_06 |
| ORD ID | ord-1e9893abe1124948b0e43289191a8e96 |
| Source note | uspto-grants-2005_06 |