Water → HCID 178489128、化合物

HRID 555960

反応式

HRID 555960 の反応式
[NH2:1][NH:2][C:3]([NH2:5])=[O:4].C([O-])(=O)C.[Na+].[CH3:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([C:19](=O)[C:20]([C:22]2[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=2)=O)=[CH:15][CH:14]=1.O>C(O)(=O)C>[OH:4][C:3]1[N:2]=[N:1][C:20]([C:22]2[CH:27]=[CH:26][C:25]([O:28][CH3:29])=[CH:24][CH:23]=2)=[C:19]([C:16]2[CH:15]=[CH:14][C:13]([O:12][CH3:11])=[CH:18][CH:17]=2)[N:5]=1

参加物

6

反応物 4

HCID 962WaterHCID 5196SemicarbazideHCID 710434,4'-DimethoxybenzilHCID 517045Sodium Acetate

生成物 1

HCID 178489128HCID 178489128、化合物収率 95%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Semicarbazide chlorohydrate (2.22 g, 20 mmol) and sodium acetate (1.80 g, 22 mmol) are added to a solution of 1,2-bis(4-methoxyphenyl)-ethane-1,2-dione (5.4 g, 20 mmol) prepared according to example 1 in acetic acid (25 ml). The mixture is heated at reflux for 12 hours. After returning to ambient temperature, the reaction mixture is poured into water. The raw reaction product is collected by filtration and washed with water. The residue is recrystallized in acetic acid. After filtration and washing in water, 5.9 g (95%) of a yellow solid is obtained after drying. δH (200 MHz, CDCl3), 3.86 (s; 6H), 6.94 (m; 4H), 7.67 (s; 4H).

後処理

  1. customprepared
  2. temperatureThe mixture is heated
  3. temperatureat reflux for 12 hours
  4. customAfter returning to ambient temperature
  5. customThe raw reaction product
  6. filtrationis collected by filtration
  7. washwashed with water
  8. customThe residue is recrystallized in acetic acid
  9. filtrationAfter filtration
  10. washwashing in water

出典と根拠

ORDレコード
ord-d30614c92eb14bd9a914fd8da32fb25d
出典データセット
uspto-grants-2011_11
特許番号
US08053573B2

関連ノート

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