HuagongsheHuagongshe Chemistry Print Report · For research reference only
Allyl bromide → HCID 22292792, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Allyl bromide | HCID 7841 | — |
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | N-Trifluoroacetyl-7-hydroxy-8-iodo-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine | HCID 22292815 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 22292792 | HCID 22292792 | 69.8% |
Reaction Steps
A solution of N-trifluoroacetyl-7-hydroxy-8-iodo-1-methyl-2,3,4,5-tetrahydro-1H-3-benzazepine (30 mg, 0.075 mmol) in dichloromethane (2 mL) was treated with allyl bromide (18 mg, 0.15 mmol), DBU (23 mg, 0.15 mmol) and stirred 2 hours at 20 C. to The product mixture was diluted with EtOAc (10 mL), washed with 5% aqueous HCl (5 mL), brine (5 mL), dried with Na2SO4 and concentrated. Flash chromatography (15% EtOAc in hexane, silica) resulted in 23 mg of a clear oil. MS calculated for C16H17F3INO2+H: 440, observed: 440.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846906B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-7f2fc08d177f4ceea68c3a9d71e3837f |
| Source note | uspto-grants-2014_09 |