Water → HCID 11148234, compound
Reaction equation
[Cl:1][CH2:2][C:3](=[O:8])[CH2:4][C:5](Cl)=[O:6].O>ClCCl.FC(F)(F)S([O-])(=O)=O.[Sc+3].FC(F)(F)S([O-])(=O)=O.FC(F)(F)S([O-])(=O)=O>[Cl:1][CH2:2][C:3]1[O:8][C:3]([CH2:2][Cl:1])=[CH:4][C:5](=[O:6])[CH:4]=1Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
4-Chloroacetoacetyl chloride (14.8 g, 33.4 mol) in dichloromethane (35% strength solution) and scandium trifluoromethanesulphonate (1.45 g, 2.5 mol) were stirred at 25° C. for 6.5 days under a nitrogen atmosphere. Water (10 g, 0.55 mol) was then added and the organic phase was concentrated. 4.2 g of product were obtained (according to GC 68% crude product). After chromatography on a silica gel column, 0.7 g of pure product corresponding to a yield of 10.8% were obtained.
Workup
- concentrationthe organic phase was concentrated
Sources & evidence
- ORD record
- ord-b2811d885fc549a398272922e21d9906
- Source dataset
- uspto-grants-2004_04
- Patent number
- US06716999B2
Reaction notes
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