HuagongsheHuagongshe Chemistry Print Report · For research reference only
9-Fluorenylmethyl chloroformate → HCID 71246275, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 9-Fluorenylmethyl chloroformate | HCID 34367 | — |
| Reactant | HCID 71246677 | HCID 71246677 | — |
| Solvent | Sodium Carbonate | HCID 10340 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 71246275 | HCID 71246275 | 98% |
Reaction Steps
219 mg (0.95 mmol, 1 eq) of (−)-[5-(8-aza-bicyclo[3.2.1]oct-6-yl)-pyridine-2-yl]-dimethylamine (VII-1) are dissolved in 1.8 ml of dioxane and 2.75 ml of 10% sodium carbonate solution. 257 mg (1 mmol, 1.05 eq) of Fmoc-Cl in portions is added and it is stirred for 1 h at RT. After this time it is diluted with EE and washed with water. The aqueous phase is re-extracted for three times with EE. The combined organic phases are dried over sodium sulphate and the solvent is removed in vacuo. The crude product is purified by column chromatography (EE:hex=1:2). 422 mg (0.93 mmol, 98%) of a colorless foam/solid is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09428497B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-2422297ea9d74a8d9db0dc8f7f2372fc |
| Source note | uspto-grants-2016_08 |