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Acetic Acid → HCID 131722517、化合物

HRID 324425
ノート
印刷プレビュー

反応式

HRID 324425 の反応式
O[N:2]=[C:3]([C:9](=[O:19])[CH2:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH3:18])[CH:13]=1)[C:4]([O:6][CH2:7][CH3:8])=[O:5].O.[C:21](O)(=[O:23])[CH3:22]>C(OC(=O)C)(=O)C.[Zn]>[C:21]([NH:2][CH:3]([C:9](=[O:19])[CH2:10][CH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH3:18])[CH:13]=1)[C:4]([O:6][CH2:7][CH3:8])=[O:5])(=[O:23])[CH3:22]
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 3

HCID 176Acetic AcidHCID 962WaterHCID 178472910HCID 178472910、化合物

生成物 1

HCID 131722517HCID 131722517、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 7918Acetic Anhydride溶媒

実験手順

Zinc dust (10 micron, 150 g) was added portionwise to a stirred solution of the product from step (i) (88 g) in acetic acid (400 ml) and acetic anhydride (125 ml) keeping the internal temperature below 40° C. The solution was stirred at room temperature for a further 1 hour before adding water (500 ml) dropwise at such a rate so as to keep the internal temperature below 40° C. The mixture was stirred at room temperature for a further 16 h then filtered and the mother liquor extracted with chloroform. The organic extracts were further washed with brine and water, collected dried over magnesium sulphate and solvent removed under reduced pressure to give the subtitle product.

後処理

  1. customthe internal temperature below 40° C
  2. customthe internal temperature below 40° C
  3. stirringThe mixture was stirred at room temperature for a further 16 h
  4. filtrationthen filtered
  5. extractionthe mother liquor extracted with chloroform
  6. washThe organic extracts were further washed with brine and water
  7. customcollected
  8. dry with materialdried over magnesium sulphate and solvent
  9. customremoved under reduced pressure

出典と根拠

ORDレコード
ord-47efe3e81ebb4afdbb546a408f16978d
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06218376B1

反応ノート

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