Dimethylformamide → HCID 53906508, compound
Reaction equation
[OH:1][C:2]1[CH:21]=[CH:20][C:5]2[C:6](=[O:19])[C:7](=[CH:9][C:10]3[CH:18]=[CH:17][C:16]4[O:15][CH2:14][O:13][C:12]=4[CH:11]=3)[O:8][C:4]=2[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>C(OCC)(=O)C>[CH2:21]([O:1][C:2]1[CH:21]=[CH:20][C:5]2[C:6](=[O:19])[C:7](=[CH:9][C:10]3[CH:18]=[CH:17][C:16]4[O:15][CH2:14][O:13][C:12]=4[CH:11]=3)[O:8][C:4]=2[CH:3]=1)[CH2:2][CH2:3][CH3:4]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
After 6-hydroxy-2-piperonylidene-3(2H)-benzofuranone 1 g and potassium carbonate 1.95 g were added to dimethylformamide 10 ml, butane 1-iodide 0.70 ml was added, and the mixture was reacted at a temperature of 100° C. for two hours. After the solution was cooled to room temperature, ethyl acetate 200 ml was added. The ethyl acetate solution was washed with water 100 ml twice and a saturated sodium chloride solution 50 ml twice. The ethyl acetate solution was dehydrated with anhydrous magnesium sulfate, and concentrated to 10 ml under reduced pressure. The precipitated crystals were filtered and dried over phosphorous pentoxide at a temperature of 60° C. for four hours under reduced pressure to obtain the desired compound 0.84 g.
Workup
- additionwas added
- customthe mixture was reacted at a temperature of 100° C. for two hours
- washThe ethyl acetate solution was washed with water 100 ml twice
- concentrationconcentrated to 10 ml under reduced pressure
- filtrationThe precipitated crystals were filtered
- dry with materialdried over phosphorous pentoxide at a temperature of 60° C. for four hours under reduced pressure
Sources & evidence
- ORD record
- ord-28c0b8872a284feb9dadb434130efbb0
- Source dataset
- uspto-grants-2000_11
- Patent number
- US06143779
Reaction notes
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