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HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 2271070Generated: November 1, 2026

Methyl iodide → HCID 9903958, compound

https://huagongshe.com/reaction/2271070

Reaction equation

Participants

RoleNameHCIDCharge
ReactantMethyl iodideHCID 6328—
ReactantSodium hydrideHCID 24758—
ReactantHCID 15434529HCID 15434529—
SolventDimethylacetamideHCID 31374—
ProductHCID 9903958HCID 990395874.8%

Reaction Steps

A solution of 0.81 g (3 mmol) of 3-fluoro-5-(N-ethylsulfonylamino)-6,7,8,9-tetrahydro-5H-benzocycloheptene (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

DOI10.6084/m9.figshare.5104873.v1
Patent numberUS06333349B1
Source datasetuspto-grants-2001_12
ORD IDord-8958c99a7ee34f06985560a64bc25e6f
Source noteuspto-grants-2001_12