HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 59485675, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 68704566 | HCID 68704566 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 59485675 | HCID 59485675 | 98.7% |
Reaction Steps
To the diamine (440 mg, 0.98 mmol) from Step 2, and triethylamine (330 μL, 2.4 mmol) in THF (20 mL) is added triphosgene (180 mg, 0.6 mmol) in THF at 0° C. After complete addition, the mixture is quenched with water and THF is removed by evaporation. The residue is extracted with ethyl acetate and washed with water. Evaporation of the organics gives a solid which is triturated with ethyl acetate, filtered, and washed with 40% ethyl acetate/hexane to give 279 mg of the title compound. Purification of the filtrate gives an additional 127 mg of product (combined yield, 88%). HPLC-MS calculated for C28H23ClN2O3 (M+H+): 471.1, found 471.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08431607B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-c1316b724b89436dad8c8559831bb947 |
| Source note | uspto-grants-2013_04 |