HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → 2-(1,1-Dioxo-1lambda6-thiomorpholin-4-yl)-7-methyl-4-p-tolyl-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 46202640 | HCID 46202640 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 2-(1,1-Dioxo-1lambda6-thiomorpholin-4-yl)-7-methyl-4-p-tolyl-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine | HCID 46202641 | 16.2% |
Reaction Steps
A mixture of 2-(1,1-dioxo-1λ6-thiomorpholin-4-yl)-4-p-tolyl-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine (0.060 g, 0.00016 mol), iodomethane (0.015 mL, 0.00016 mol) and N-ethyl-N-(1-methylethyl)-2-propanamine (0.056 mL, 0.00032 mol) in DCM (2 mL) was stirred at rt for 3 h. The mixture was diluted with DCM and washed with water (3×) and satd. aq. NaCl. The separated organic layer was dried and concentrated. The residue was purified by FCC [7 N NH3/MeOH)/DCM] to give 0.010 g (16%) of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08829011B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-e990197c8c5d464686f8c1b6b62ba4cd |
| Source note | uspto-grants-2014_09 |