HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Methyl-2-butanone → 4,5,6-triiodo-2,3,3-trimethyl-3H-indole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Methyl-2-butanone | HCID 11251 | — |
| Reactant | 3,4,5-Triiodophenylhydrazine | HCID 86695333 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 4,5,6-triiodo-2,3,3-trimethyl-3H-indole | HCID 71736008 | 27.1% |
Reaction Steps
2 g of 3,4,5-triiodophenylhydrazine, and 0.86 g (10 mmol) of 3-methyl-2-butanone were refluxed in 15 mL of acetic acid for 16 hours. The acetic acid was evaporated, the residue was dissolved in chloroform, washed with aqueous solutions of NaHCO3, followed by Na2S2O3 and water. The organic layer was dried and chloroform was removed under reduced pressure by a rotary evaporator. The residue was column purified (Silica gel 60, 0-2% methanol-chloroform) to give 0.6 g of 4,5,6-triiodo-2,3,3-trimethyl-3H-indole. 1H-NMR (200 MHz, DMSO-d6), δ, ppm: 8.04 (1H, s, arom.), 2.19 (3H, s, 2-CH3), 1.30 (6H, s, C(CH3)2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09040721B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-e2c414c7cd424c71a2549700318ad144 |
| Source note | uspto-grants-2015_05 |