HCID 131726643, compound → Benzil monoxime
Reaction equation
C(O)(=O)C=C.[C:6]1([C:12](=[N:21][OH:22])[C:13]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[O:14])[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>C(Cl)(Cl)Cl>[C:6]1([C:12](=[N:21][OH:22])[C:13]([C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)=[O:14])[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1Participants
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
As shown in the following reaction 1, 30 g of benzil monoxime acrylate, which is obtained from the reaction of benzil monoxime and chloroacylate, and 1 L of chloroform were added into a 2 L reactor, and was stirred and cooled in iced water. 47 g of 3-chloroperoxybenzoicacid(mCPBA) were slowly added into the cooled solution, and the reaction was carried out at room temperature for 24 hours. After completion of the reaction, the 3-chlorobenzoicacid (by-product) was removed by filtering the product, and then the residual 3-chlorobenzoicacid was removed by washing 2 times with saturated sodium sulfite aqueous solution, 1 time with saturated sodium bicarbonate aqueous solution, 1 time with saturated sodium chloride aqueous solution, and 1 time with distilled water. Next, the product was dried with magnesium sulfate, and chloroform was removed under reduced pressure, and then the product was vacuum dried for 1 day to obtain 25.5 g of the pure benzil monoxime acrylate oxide. NMR spectrum of the obtained benzil monoxime acrylate oxide is described in FIG. 1.
Sources & evidence
- ORD record
- ord-baffb067dbde47ed912108b725b768c2
- Source dataset
- uspto-grants-2007_10
- Patent number
- US07282530B2
Reaction notes
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