HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 68469260, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 68469873 | HCID 68469873 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 68469260 | HCID 68469260 | — |
Reaction Steps
3.39 g (14.0 mmol) ethyl (S)-4-hydroxy-4,5,7,8-tetrahydro-thieno[2,3-d]azepine-6-carboxylate in 40 ml THF are mixed batchwise with 0.86 g of 60% NaH mineral oil dispersion while cooling with an ice bath, the mixture is stirred for 15 min and then 1.07 ml methyl iodide are slowly added dropwise. The mixture is stirred for 1 h, poured onto ice water and extracted 3× with ethyl acetate. The combined organic phases are dried with NaSO4 and concentrated.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08309542B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-7c5ae49147834b0892b00fa4f8306346 |
| Source note | uspto-grants-2012_11 |