HuagongsheHuagongshe Chemistry Print Report · For research reference only
Calcium Carbonate → HCID 58495417, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Calcium Carbonate | HCID 10112 | — |
| Reactant | Trimethylbenzylammonium Dichloroiodate | HCID 56924451 | — |
| Reactant | HCID 70667124 | HCID 70667124 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58495417 | HCID 58495417 | 82.2% |
Reaction Steps
To a mixed solution of 770 mg of t-butyl[2-(1,2,3,4-tetrahydroquinolin-7-yl)ethyl]carbamate in 15 ml of dichloromethane and 3 ml of MeOH were added 420 mg of calcium carbonate and 970 mg of benzyltrimethylammonium dichloroiodate, followed by stirring at room temperature for 2 hours. The insoluble materials were removed by filtration and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel chromatography (elution solvent: HEX-EtOAc) to obtain 595 mg of t-butyl [2-(6-iodo-1,2,3,4-tetrahydroquinolin-7-yl)ethyl]carbamate as a reddish brown viscous substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09108977B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-a2886995a72a4cf2a05aaab9e92eb085 |
| Source note | uspto-grants-2015_08 |