HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 57535429, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Reactant | HCID 57535415 | HCID 57535415 | — |
| Solvent | Acetic acid methylene chloride | HCID 21922555 | — |
| Product | HCID 57535429 | HCID 57535429 | — |
Reaction Steps
To the amino from step 2 (1.0 eq) in CH2Cl2—AcOH (1:1) at −20° C. was added iodine (1.5 eq), KI (1.5 eq) followed by NaNO2 (1.2 eq). The reaction mixture was stirred at r.t. for 1 h, diluted with EtOAc, a solution of Na2CO3 and a solution Na2S2O3. The organic extracts were washed with water, brine, dried over MgSO4, filtered and concentrated. Flash chromatography (Hexane:EtOAc, 30:20-20:30) afforded the title compound as a pale yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07482456B2 |
| Source dataset | uspto-grants-2009_01 |
| ORD ID | ord-db9ec7ca692246bd858b6b473c7cb139 |
| Source note | uspto-grants-2009_01 |