HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → HCID 59441746, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 59442091 | HCID 59442091 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59441746 | HCID 59441746 | — |
Reaction Steps
1-[3-(methyloxy)-4-nitrophenyl]hexahydro-1H-1,4-diazepine (as the TFA salt) (1.0 g, 2.08 mmol) was dissolved in dichloromethane (10 mL) and triethylamine (0.87 mL, 6.25 mmol). Methanesulfonyl chloride (0.24 mL, 3.12 mmol) was added slowly and stirred at rt for 30 min. At this time the reaction mixture was diluted with dichloromethane and washed with a saturated bicarbonate solution, water and a saturated sodium chloride solution, dried over Na2SO4 and filtered. Solvents were removed under reduced pressure to afford 1-[3-(methyloxy)-4-nitrophenyl]-4-(methylsulfonyl)hexahydro-1H-1,4-diazepine. (0.737 g, 2.24 mmol) as a yellow/brown solid. ESIMS (M+H)+=330.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07981903B2 |
| Source dataset | uspto-grants-2011_07 |
| ORD ID | ord-44275c52cac748dbb112f9f1665dff0e |
| Source note | uspto-grants-2011_07 |