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Acetic Acid → HCID 131722520、化合物

HRID 324443
ノート
印刷プレビュー

反応式

HRID 324443 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH2:8][CH2:9][C:10](=[O:19])[C:11](=[N:17]O)[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:5]=[CH:6][CH:7]=1.O.[C:21](O)(=[O:23])[CH3:22]>C(OC(=O)C)(=O)C.[Zn]>[C:21]([NH:17][CH:11]([C:10](=[O:19])[CH2:9][CH2:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=1)[C:12]([O:14][CH2:15][CH3:16])=[O:13])(=[O:23])[CH3:22]
参加物反応条件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 178472912HCID 178472912、化合物

生成物 1

HCID 131722520HCID 131722520、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 7918Acetic Anhydride溶媒

反応条件

温度
40 °C

実験手順

To a stirred solution of the product from step (ii) in acetic acid (125 ml) and acetic anhydride (40 ml) was added zinc dust (45 g) portionwise at a rate to maintain the internal temperature <40° C. The mixture was stirred for 30 min and water (125 ml) was added at such a rate as to maintain the temperature at around 40° C. The mixture was stirred at room temperature for 2 hours and filtered. The mother liquor was extracted with dichloromethane and further washed with water. The organic layer was collected, dried (MgSO4) and solvent evaporated under reduced pressure to give the subtitle product.

後処理

  1. temperatureto maintain the internal temperature <40° C
  2. stirringThe mixture was stirred at room temperature for 2 hours
  3. filtrationfiltered
  4. extractionThe mother liquor was extracted with dichloromethane
  5. washfurther washed with water
  6. customThe organic layer was collected
  7. dry with materialdried (MgSO4) and solvent
  8. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-929d8174cd0040a28be49daa704866ea
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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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート