Water → HCID 178489128, 화합물

HRID 555960

반응식

HRID 555960 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 178489128HCID 178489128, 화합물수율 95%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d30614c92eb14bd9a914fd8da32fb25d
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08053573B2

연결된 노트

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