HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 28492569, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | 5-Bromoisatin | HCID 6889 | — |
| Reactant | o-Xylyl bromide | HCID 6992 | — |
| Reactant | 2-((1,1-Dimethylethyl)imino)-N,N-diethylhexahydro-1,3-dimethyl-2lambda5-1,3,2-diazaphosphorin-2-amine | HCID 3513851 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 28492569 | HCID 28492569 | 53% |
Reaction Steps
Combine 5-bromoisatin (90 mg, 0.4 mmol), 2-tert-butylimino-2-diethylamino-1,3-dimethyl-perhydro-1,3,2-diazaphosphorine on polysteyrene (270-290 mg, 0.60-0.64 mmol, 2.2 mmol/g, Fluka) and 2-methylbenzyl bromide (0.054 mL, 0.4 mmol) in acetonitrile (4 mL) in a 20 dram scintillation vial and shake on a rotator for 2.5 days. Dilute with and a small amount of CH2Cl2 as needed to soluabilize solids. Filter off beads, washing with MeOH, and concentrate in vacuo. Triturate the resulting solid with diethyl ether (about 4 mL) and pipet off the liquid. Dry the solid to obtain approximately 70 mg of the title compound as crude material and use without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07250442B2 |
| Source dataset | uspto-grants-2007_07 |
| ORD ID | ord-61bcf6830bd24818b80c74810c7137b1 |
| Source note | uspto-grants-2007_07 |