HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 15950100, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Trimethylsilyl iodide | HCID 85247 | — |
| Reactant | HCID 58017135 | HCID 58017135 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 15950100 | HCID 15950100 | — |
Reaction Steps
Alternatively, a solution of methyl [5-chloro-1′-(3-chlorobenzyl)-2,2′,5′-trioxospiro[indole-3,3′-pyrrolidin]-1(2H)-yl)acetate, intermediate 48, (250 mg, 0.56 mmol) in chloroforme or acetonitrile (10 ml) was treated with iodotrimethylsilane (0.31 ml, 2.24 mmol) and heated up to reflux until completion. Addition of 1.0 N HCl (10 ml), product extraction with ethyl acetate or chloroforme (3×5 ml), washing of the combined extracts with sat. sodium thiosulfate (10 ml) and drying (MgSO4) gave the title compound as in quant.yield as slightly yellow solid (75% purity by HPLC using chloroform; 68% purity by HPLC using acetonitrile). MS (ESI+): 434.3; MS (ESI−): 431.4.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08236963B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-d4d1731a92d0450686fbb965be41d5a6 |
| Source note | uspto-grants-2012_08 |