HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 22479029, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | HCID 12264703 | HCID 12264703 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 22479029 | HCID 22479029 | 72.7% |
Reaction Steps
A solution of 1.0 g of 1,2,3,4-tetrahydro-6,7-dimethoxy-4,4-dimethyl-isoquinoline in 100 ml of ethanol is treated with 2.3 g of iodine and 0.49 g of sodium acetate and heated under reflux for 1 hour. The reaction mixture is cooled down and 30 ml of a 10% sodium thiosulphate-solution is added. The mixture is then diluted with water and extracted with dichloromethane (2×100 ml). The combined organic extracts are washed with brine, dried over sodium sulfate and concentrated in vacuo. The foamy residue is purified by chromatography (SiO2, dichloromethane-1% ammonia in methanol, 0-12%) to give the title compound as a yellowish oil (0.72 g), MS (ISP) 220.4 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06727261B2 |
| Source dataset | uspto-grants-2004_04 |
| ORD ID | ord-3093c2860cd74b738026a8ff00bcefc5 |
| Source note | uspto-grants-2004_04 |