HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 10274041, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | 2-Dimethylaminopyridine | HCID 21885 | — |
| Reactant | 1-(1,3-benzodioxol-5-yl)-2,3,4,9-tetrahydro-1H-beta-carboline | HCID 201172 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10274041 | HCID 10274041 | — |
Reaction Steps
To a solution of 1-(3,4-methylenedioxyphenyl)-2,3,4,9-tetrahydro-1H-β-carboline (9.11 g, 31.1 mmol) (prepared according to the process as disclosed in WO97/43287, Intermediate 7, page 24) in dry dichloromethane (100 mL) were added triethylamine (8.80 mL, 63.1 mmol) and dimethylaminopyridine (5 mg), followed by the dropwise addition of benzylchloroformate (4.60 mL, 30.6 mmol) over a period of 30 min. The reaction mixture was stirred for 16 h, transferred to a separatory funnel, washed with 2N HCl, brine, dried over anhydrous magnesium sulfate and concentration in vacuo. Flash chromatography yielded the product as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06818646B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-e494bc2b4c704573aad168112baea252 |
| Source note | uspto-grants-2004_11 |