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Oxalic Acid → HCID 15034422、化合物

HRID 1073855
ノート
印刷プレビュー

反応式

HRID 1073855 の反応式
C([O:3][CH:4](OCC)[CH2:5][O:6][C:7]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:8]=1[O:14][CH3:15])C.C(O)(=O)C(O)=O>CC(C)=O>[F:13][C:11]1[CH:10]=[CH:9][C:8]([O:14][CH3:15])=[C:7]([CH:12]=1)[O:6][CH2:5][CH:4]=[O:3]
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 971Oxalic AcidHCID 15079980HCID 15079980、化合物

生成物 1

HCID 15034422HCID 15034422、化合物収率 30.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 23.0 g of 2-(5-fluoro-2-methoxyphenoxy)acetaldehyde diethylacetal in 130 ml of acetone were added 100 ml of 10% aqueous oxalic acid and the mixture was refluxed for 2 hours. After cooling, the reaction mixture was evaporated, and the residue was diluted with water and extracted with ether. The extract was washed with water, dried and evaporated. Isopropyl ether was added to the residue and the precipitate was filtered to give 4.99 g of the desired compound as pale brown crystals, which were recrystallized from a mixture of isopropanol and isopropyl ether as pale brown crystals, m.p. 92.5°-95° C.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. temperaturethe mixture was refluxed for 2 hours
  2. temperatureAfter cooling
  3. customthe reaction mixture was evaporated
  4. additionthe residue was diluted with water
  5. extractionextracted with ether
  6. washThe extract was washed with water
  7. customdried
  8. customevaporated
  9. additionIsopropyl ether was added to the residue
  10. filtrationthe precipitate was filtered

出典と根拠

ORDレコード
ord-1952c50c855f453cb5d10af57b0d5218
出典データセット
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04971990

反応ノート

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