HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → HCID 18439222, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Trimethylsilyldiazomethane | HCID 167693 | — |
| Reactant | HCID 18439217 | HCID 18439217 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 18439222 | HCID 18439222 | — |
Reaction Steps
In a 3-neck 250 mL round-bottom flask fitted with a thermometer and a condenser, 3-methoxy-2,4,6-triiodobenzoic acid (10.38 g) was dissolved in a 2:1 mixture of Et2O and methanol at 0° C. A 2.0 M hexanes solution of TMSCHN2 was added dropwise until yellow color persisted and N2 bubbling stopped. The reaction mixture was stirred for 30 minutes and quenched with glacial acetic acid. Solvents and excess AcOH were removed in vacuo for 18 h to give the desired ester as a white solid which was used in the next step without any further purification. Yield 11.07 g (˜100% crude).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07186797B2 |
| Source dataset | uspto-grants-2007_03 |
| ORD ID | ord-c9486bf3be634bfbbec14a7afafac660 |
| Source note | uspto-grants-2007_03 |