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Sulfuric acid magnesium salt (1:1) → 2-({2-[(5,6-dihydro-[1,4,2]dioxazin-3-yl)-methoxyimino-methyl]-benzylidene}-hydrazono)-1-phenylpropan-1-one O-methyl oxime

HRID 2229130
ノート
印刷プレビュー

反応式

HRID 2229130 の反応式
[CH3:1][O:2][N:3]=[C:4]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:5](=[N:7][NH2:8])[CH3:6].[O:15]1[CH2:20][CH2:19][O:18][C:17]([C:21](=[N:30][O:31][CH3:32])[C:22]2[CH:29]=[CH:28][CH:27]=[CH:26][C:23]=2[CH:24]=O)=[N:16]1.S([O-])([O-])(=O)=O.[Mg+2]>C(O)C>[CH3:1][O:2][N:3]=[C:4]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:5](=[N:7][N:8]=[CH:24][C:23]1[CH:26]=[CH:27][CH:28]=[CH:29][C:22]=1[C:21]([C:17]1[O:18][CH2:19][CH2:20][O:15][N:16]=1)=[N:30][O:31][CH3:32])[CH3:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 542963122-[(5,6-Dihydro-[1,4,2]dioxazin-3-yl)-methoxyimino-methyl]-benzaldehydeHCID 572718472-hydrazono-1-phenylpropan-1-one O-methyl oxime

生成物 1

HCID 725917742-({2-[(5,6-dihydro-[1,4,2]dioxazin-3-yl)-methoxyimino-methyl]-benzylidene}-hydrazono)-1-phenylpropan-1-one O-methyl oxime収率 41.1%

試薬・触媒・溶媒 1

HCID 702
Ethanol
溶媒

実験手順

1 g (0.0052 mol) of 2-hydrazono-1-phenylpropan-1-one O-methyl oxime is heated under reflux at the boiling point in 5 ml of ethanol with 1.3 g (0.0052 mol) of 2-[(5,6-dihydro-[1,4,2]dioxazin-3-yl)-methoxyimino-methyl]-benzaldehyde and 5 g of anhydrous magnesium sulphate for 1 hour. The reaction mixture is poured onto water and extracted with diethyl ether, the organic phase is dried over sodium sulphate and the solvent is distilled off in vacuo. The residue is stirred with diethyl ether and the crystals formed are filtered off. The solid is chromatographed over silica gel with diethylether/petroleum ether/methylene chloride (2:1:1). 0.9 g (40.8% of theory) of crystalline 2-({2-[(5,6-dihydro-[1,4,2]dioxazin-3-yl)-methoxyimino-methyl]-benzylidene}-hydrazono)-1-phenylpropan-1-one O-methyl oxime of melting point 136° C. is obtained.

後処理

  1. additionThe reaction mixture is poured onto water
  2. extractionextracted with diethyl ether
  3. dry with materialthe organic phase is dried over sodium sulphate
  4. distillationthe solvent is distilled off in vacuo
  5. customthe crystals formed
  6. filtrationare filtered off
  7. customThe solid is chromatographed over silica gel with diethylether/petroleum ether/methylene chloride (2:1:1)

出典と根拠

ORDレコード
ord-a385d8404f66438298dafa7c5595ac41
出典データセット
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06420362B1

反応ノート

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