HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-Trifluoroacetyl-1,2,4,5-tetrahydro-3-benzazepine-7-sulfonyl fluoride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Acetonitrile | HCID 6342 | — |
| Reactant | Potassium Fluoride | HCID 522689 | — |
| Reactant | 3-Trifluoroacetyl-1,2,4,5-tetrahydro-3-benzazepine-7-sulfonyl chloride | HCID 54286576 | — |
| Catalyst | 18-Crown-6 | HCID 28557 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 3-Trifluoroacetyl-1,2,4,5-tetrahydro-3-benzazepine-7-sulfonyl fluoride | HCID 57592483 | 96.4% |
Reaction Steps
A mixture of 3-trifluoroacetyl-2,3,4,5-tetrahydro-1H-3-benzazepine-7-sulfonyl chloride (23 g, 67 mmol), potassium fluoride (12 g, 200 mmol), 18-crown-6 (0.1 g), and acetonitrile (100 mL) was stirred overnight. Water (200 mL) and ethyl acetate (200 mL) were added and the organic layer was washed with brine (100 mL), dried (MgSO4), and evaporated to give the title compound D1 as a white solid (21 g). 1H NMR 3 (d6-DMSO) 3.2 (4H, m), 3.7 (4H, m), 7.6 (1H, m), and 8.0 (2H, m).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07504392B2 |
| Source dataset | uspto-grants-2009_03 |
| ORD ID | ord-d21019d42db04134bf3db7424f83b87b |
| Source note | uspto-grants-2009_03 |