HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphosgene → 1-Methoxy-3-(methoxymethoxy)benzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | N1-{6-[(3-ethyl-1,3-dihydro-2-benzofuran-4-yl)oxy]-3-pyridinyl}-2-methylalaninamide | HCID 86698445 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 1-Methoxy-3-(methoxymethoxy)benzene | HCID 542621 | 791% |
| Product | 3-{6-[(3-Ethyl-1,3-dihydro-2-benzofuran-4-yl)oxy]-3-pyridinyl}-5,5-dimethyl-2,4-imidazolidinedione | HCID 57410827 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
In a 50 mL round-bottomed flask N1-{6-[(3-ethyl-1,3-dihydro-2-benzofuran-4-yl)oxy]-3-pyridinyl}-2-methylalaninamide (Intermediate 149, 17.2 mg, 0.050 mmol) was dissolved in Dichloromethane (3 mL) to give a pale yellow solution that was cooled at 0° C. TEA (0.035 mL, 0.252 mmol) was added followed by a dropwise addition of a solution of triphosgene (6.43 mg, 0.023 mmol) in dichloromethane (0.5 ml) and the reaction mixture was stirred at 0° C. for 20 minutes. The reaction mixture was evaporated in vacuo and the residue was purified by flash chromatography (Biotage system) on silica gel using a column SNAP 10 g and cyclohexane/ethyl acetate from 2:1 to 1:2 as eluents affording the title compound Example 45 (15.3 mg) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09346790B2 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-f3a5987a4aac41a9a15da8417ba1d550 |
| Source note | uspto-grants-2016_05 |