Hydrochloric Acid → HCID 15882750, compound
Reaction equation
Br[CH2:2][C:3]1[C:4]([O:6][C:7](=[O:10])[C:8]=1[CH3:9])=[O:5].[OH-:11].[Na+].Cl.[Cl-].[Na+]>CCCCCC.C(OCC)(=O)C>[OH:11][CH2:2][C:3]1[C:4]([O:6][C:7](=[O:10])[C:8]=1[CH3:9])=[O:5]Participants
6
Reactant 4
Product 1
Reagents, catalysts & solvents 1
Procedure
To 2-bromomethyl-3-methylmaleic anhydride (1.25 g, 6.10 mmol) was added 5 M aqueous sodium hydroxide solution (4 mL) at room temperature, and the mixture was stirred for 12 h. The reaction mixture was adjusted to pH 1 with 5 M hydrochloric acid (5 mL), added with sodium chloride and extracted three times with ethyl acetate. The combined organic layer was concentrated under reduced pressure, and the residue thus obtained was subjected to silica gel column chromatography (hexane-ethyl acetate 2:1) to give 227 mg of the title compound as oil (yield: 26%).
Workup
- extractionextracted three times with ethyl acetate
- concentrationThe combined organic layer was concentrated under reduced pressure
- customthe residue thus obtained
Sources & evidence
- ORD record
- ord-173cf8a3b8654c6c8296c446c42b1cb9
- Source dataset
- uspto-grants-2012_01
- Patent number
- US08093294B2
Reaction notes
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