Hydrochloric Acid → HCID 22417098, compound
Reaction equation
[F:1][C:2]1[C:3]([F:18])=[C:4](F)[C:5]([F:16])=[C:6]([C:12]([O:14][CH3:15])=[O:13])[C:7]=1[C:8]([O:10][CH3:11])=[O:9].C1CCN2C(=NCCC2)CC1.Cl.[N+:31]([CH3:34])([O-:33])=[O:32]>>[F:16][C:5]1[C:4]([CH2:34][N+:31]([O-:33])=[O:32])=[C:3]([F:18])[C:2]([F:1])=[C:7]([C:8]([O:10][CH3:11])=[O:9])[C:6]=1[C:12]([O:14][CH3:15])=[O:13]Participants
5
Conditions
- Temperature
- 10 °C
Procedure
200 g of dimethyl tetrafluorophthalate was dissolved in 400 ml of nitromethane (Ishikawa, Suzuki & Tanabe: Nippon Kagaku Kaishi, 1976, 200) and the solution was cooled on an ice-salt bath. At an internal temperature of 15°-20° C., 171 g of 1,8-diazabicyclo[5,4,0]-7-undecene was added dropwise over a period of 30 minutes. After completion of the dropwise addition, the mixture was further stirred at an internal temperature of 10° C. for 30 minutes, then, the mixture was poured into a mixture of 1.5 liters of 1N hydrochloric acid and 1 liter of ice.
Workup
- temperaturethe solution was cooled on an ice-salt bath
- additionAfter completion of the dropwise addition
Sources & evidence
- ORD record
- ord-3ce6924ff1434b7fb38471ae5cf621b8
- Source dataset
- uspto-grants-1994_02
- Patent number
- US05286723
Reaction notes
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