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Cyanuric chloride → Acetone, O,Oa(2),Oa(2)a(2)-s-triazine-2,4,6-triyltrioxime

HRID 1773845
ノート
印刷プレビュー

反応式

HRID 1773845 の反応式
[CH3:1][C:2](=[N:4][OH:5])[CH3:3].[N:6]1[C:13](Cl)=[N:12][C:10](Cl)=[N:9][C:7]=1Cl>N1C=CC=CC=1>[C:2](=[N:4][O:5][C:7]1[N:9]=[C:10]([O:5][N:4]=[C:2]([CH3:3])[CH3:1])[N:12]=[C:13]([O:5][N:4]=[C:2]([CH3:3])[CH3:1])[N:6]=1)([CH3:3])[CH3:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7954Cyanuric chlorideHCID 67180Acetone, oxime

生成物 1

HCID 90113126Acetone, O,Oa(2),Oa(2)a(2)-s-triazine-2,4,6-triyltrioxime収率 94.8%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a cold (0° C.) solution of acetone oxime (2.92 g, 0.04 mol) in dry pyridine (15 ml) is added cyanuric chloride (1.84 g, 0.01 mol). An exothermic reaction occurs and the temperature rises to 35° C. The solution is then stirred for 5 h at room temperature and then poured into 100 ml of ice-cold water. The resulting emulsion is extracted with dichloromethane (5×20 ml), the extracts are dried over MgSO4 and the solvent is evaporated. The residue is chromatographed (silica gel, CH2Cl2—C2H5O(CO)CH3 7:3) and the pure fraction is recrystallized from dichloromethane-hexane to afford 2.79 g of the title compound as a white solid, mp. 156-158° C.

後処理

  1. customAn exothermic reaction
  2. customrises to 35° C
  3. extractionThe resulting emulsion is extracted with dichloromethane (5×20 ml)
  4. dry with materialthe extracts are dried over MgSO4
  5. customthe solvent is evaporated
  6. customThe residue is chromatographed (silica gel, CH2Cl2—C2H5O(CO)CH3 7:3)
  7. customthe pure fraction is recrystallized from dichloromethane-hexane

出典と根拠

ORDレコード
ord-5b9e4cb2188a46e0b3aa9ce06b2bfbd0
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09255217B2

反応ノート

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