HCID 131726643、化合物 → Benzil monoxime

HRID 1180617ノート

反応式

HRID 1180617 の反応式
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]=1

参加物

3

反応物 1

HCID 131726643HCID 131726643、化合物

生成物 1

HCID 6419297Benzil monoxime

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

出典と根拠

ORDレコード
ord-baffb067dbde47ed912108b725b768c2
出典データセット
uspto-grants-2007_10
特許番号
US07282530B2

反応ノート

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