HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosuccinimide → (4R,9aR)-7-Chloro-4,6-dimethyl-3,4,9,9a-tetrahydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | (R)-4,6-Dimethyl-3,4-dihydro-1H-2,4a,5-triaza-fluorene-2-carboxylic Acid Tert-butyl Ester | HCID 69357516 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | (4R,9aR)-7-Chloro-4,6-dimethyl-3,4,9,9a-tetrahydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester | HCID 69357620 | — |
Reaction Steps
To a solution of 0.20 g (0.66 mmol) (R)-4,6-dimethyl-3,4-dihydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester in 2 mL tetrahydrofuran was added 92.1 μg (0.69 mmol) N-chlorosuccinimide. The reaction was stirred at 50 deg C. for 18 h, then the solvent was evaporated and the residue was purified by column chromatography on silica gel (0.032–0.063 mm) with ethyl acetate:dichloromethane (1:19) as eluant.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07208494B2 |
| Source dataset | uspto-grants-2007_04 |
| ORD ID | ord-3aa9b957890b4570a1b952d8a8cb99f4 |
| Source note | uspto-grants-2007_04 |