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

HRID 905367
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HRID 905367 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

HCID 1317133262,6-Dichloro-3-nitrobenzylideneaminooxyacetic Acid

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-53d2f437ebe943f9bff6bf863ea181a4
출처 데이터셋
uspto-grants-1983_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04423241

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