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Ethanol → 2,6-Dichloro-3-nitrobenzylideneaminooxyacetic Acid

HRID 905367
ノート
印刷プレビュー

反応式

HRID 905367 の反応式
Cl[C:2]1[C:9]([N+:10]([O-:12])=[O:11])=[CH:8][CH:7]=[C:6]([Cl:13])[C:3]=1[CH:4]=O.C(O)C.[ClH:17].[C:18]([CH2:21][O:22][NH2:23])([OH:20])=[O:19].C(CON)(O)=O.C([O-])(=O)C.[Na+]>O>[Cl:17][CH:21]([O:22][N:23]=[CH:4][C:3]1[C:6]([Cl:13])=[CH:7][CH:8]=[C:9]([N+:10]([O-:12])=[O:11])[CH:2]=1)[C:18]([OH:20])=[O:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 702EthanolHCID 517045Sodium AcetateHCID 2723609Aminooxyacetic acid hemihydrochlorideHCID 27949122,6-Dichloro-3-nitrobenzaldehyde

生成物 1

HCID 1317133262,6-Dichloro-3-nitrobenzylideneaminooxyacetic Acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A warm solution of 2,6-dichloro-3-nitrobenzaldehyde, 1.8 gm. in 20 ml. of ethanol was stirred into a solution of 0.9 gm. (0.008 equivs.) of carboxymethoxylamine hemihydrochloride and 0.45 gm. of sodium acetate, anhyd., in 20 ml. of water at room temperature. The mixture was heated on the steam bath for one-half hour, and was then evaporated to dryness at room temperature. The residue was triturated with cold water, filtered, washed with cold water and dried in air to obtain 2.1 gm. (87.4%) of crude material melting at 76°-84° C. This was purified from aqueous-methanol to obtain 1.9 gm. of pale cream-colored product melting at 82°-85° C.

後処理

  1. customat room temperature
  2. temperatureThe mixture was heated on the steam bath for one-half hour
  3. customwas then evaporated to dryness at room temperature
  4. customThe residue was triturated with cold water
  5. filtrationfiltered
  6. washwashed with cold water
  7. customdried in air
  8. customto obtain 2.1 gm
  9. customThis was purified from aqueous-methanol
  10. customto obtain 1.9 gm

出典と根拠

ORDレコード
ord-53d2f437ebe943f9bff6bf863ea181a4
出典データセット
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04423241

反応ノート

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