HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trityl chloride → 5-Bromo-2-trityl-isoindoline
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trityl chloride | HCID 6456 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 5-Bromoisoindoline | HCID 14795871 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-Bromo-2-trityl-isoindoline | HCID 59263113 | 85.5% |
Reaction Steps
Trityl chloride (2.30 g, 8.23 mmol) was added to a solution of 5-bromo-2,3-dihydro-1H-isoindole (1.64 g, 8.23 mmol) and triethylamine (1.4 mL, 9.9 mmol) in dichloromethane (20 mL). After 18 hours the solvent was removed in vacuo, the residue taken up in ethyl acetate and washed with water (×2) and brine, dried (MgSO4) and concentrated. The crude material was purified by flash chromatography on silica eluting with 1% triethylamine/10% ethyl acetate/petrol to give 5-bromo-2-trityl-2,3-dihydro-1H-isoindole as a reddish-brown solid (3.10 g, 85%). 1H NMR (CDCl3) 7.91-7.84 (1H, m), 7.57 (6H, d), 7.45-7.41 (1H, m), 7.33-7.14 (9H, m), 6.95 (1H, d), 3.90 (2H, s), 3.86 (2H, s). MS: Ph3C+243.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08101648B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-3c6a029389d0433c8524802a8a01be98 |
| Source note | uspto-grants-2012_01 |