HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorotrimethylsilane → HCID 57470079, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorotrimethylsilane | HCID 6397 | — |
| Reactant | 1,2-Dibromoethane | HCID 7839 | — |
| Reactant | 1-Bromo-4-nitrobenzene | HCID 11466 | — |
| Reactant | Tris(furan-2-yl)phosphane | HCID 521585 | — |
| Reactant | Tert-butyl 3-iodoazetidine-1-carboxylate | HCID 11000522 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Catalyst | Bis(dibenzylideneacetone)palladium | HCID 9811564 | — |
| Product | HCID 57470079 | HCID 57470079 | 52% |
Reaction Steps
Following the same procedure as described in 46.3, the organozinc species was prepared using 3-iodo-azetidine-1-carboxylic acid tert-butyl ester (1.74 g, 6.14 mmol), Zn dust (520 mg, 7.95 mmol), 1,2 dibromoethane (84 μl, 0.97 mmol) and trimethylsilyl chloride (115 μl, 0.92 mmol). It was then coupled with 1-bromo-4-nitrobenzene (1.24 g, 6.13 mmol) using Pd2(dba)3 (90 mg, 0.10 mmol) and P(2-furyl)3 (85 mg, 0.36 mmol). Purification of the crude product by flash column chromatography (heptane:ethyl acetate, 4:1) provides the title compound (880 mg, 52%) as a light yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08470810B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-dbe0b35f63304ab385715b6e3cfcb427 |
| Source note | uspto-grants-2013_06 |