Sulfuric Acid → HCID 67099792, compound
Reaction equation
O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.OS(O)(=O)=O.[Cl:20][C:21]1[C:26]([Cl:27])=[CH:25][CH:24]=[CH:23][C:22]=1[C:28]([CH3:43])([CH3:42])[C:29]([CH:31]([C:37]([O:39][CH2:40][CH3:41])=[O:38])[C:32]([O:34]CC)=O)=[O:30]>>[Cl:27][C:26]1[C:21]([Cl:20])=[C:22]2[C:23]([C:32]([OH:34])=[C:31]([C:37]([O:39][CH2:40][CH3:41])=[O:38])[C:29](=[O:30])[C:28]2([CH3:42])[CH3:43])=[CH:24][CH:25]=1Participants
4
Conditions
- Temperature
- 25 °C
Procedure
P2O5 (5.00 g, 35 mmol) was treated with H2SO4 (4.5 mL, 81 mmol) at 0° C. in a 100 mL round bottom flask. Diethyl 2-(2-(2,3-dichlorophenyl)-2-methylpropanoyl)malonate (0.500 g, 1.0 mmol) was added, and the mixture was stirred at 25° C. for 1.5 hours. The reaction was quenched with ice, extracted with EtOAc (2×50 mL), and the combined organic layers were washed with brine (50 mL). The organic layers were then dried over MgSO4, concentrated, and dried in vacuo to give the title compound (0.235 g). MS m/e=329 (M+H)+.
Workup
- customThe reaction was quenched with ice
- extractionextracted with EtOAc (2×50 mL)
- washthe combined organic layers were washed with brine (50 mL)
- dry with materialThe organic layers were then dried over MgSO4
- concentrationconcentrated
- customdried in vacuo
Sources & evidence
- ORD record
- ord-e5cf7759a7524d9ebff91adf2533ca84
- Source dataset
- uspto-grants-2009_12
- Patent number
- US07635715B2
Reaction notes
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