HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 10193055, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | Phenol, 4-methoxy-2-nitro- | HCID 15285 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 10193055 | HCID 10193055 | 57.3% |
Reaction Steps
A solution of 4-Methoxy-2-nitrophenol (5 g, 29.6 mmol) in MeOH (100 mL) was cooled to 0° C. and treated with KOH (1.8 g, 32.6 mmol) followed by portionwise addition of I2 (8.2 g, 32.6 mmol). The reaction was worked-up by quenching the excess I2 by adding a 10% Na2SO3 aq solution. The MeOH was stripped off and 2 N HCl aq. was added and the aqueous extracted with EtOAc. The EtOAc was washed with saturated NaHCO3, brine and dried over MgSO4. The solution was concentrated and triturated twice with MeOH to yield 5 g of material that consisted of a 2:1 mixture of product to starting material that was used as is for the next step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06774248B2 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-6c9d3c16b27f44d1aab8201e75dbdb5b |
| Source note | uspto-grants-2004_08 |