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Sodium Hydroxide → 1(6H)-Pyridazinenonanoic acid, 6-oxo-3,4-diphenyl-

HRID 981475
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HRID 981475 반응식
[O:1]=[C:2]1[N:7]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([O:18]C)=[O:17])[N:6]=[C:5]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:4]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:3]1.[OH-].[Na+]>CO>[O:1]=[C:2]1[N:7]([CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=[O:17])[N:6]=[C:5]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[C:4]([C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 9931844methyl 6-oxo-3,4-diphenyl-1(6H)-pyridazinenonanoate

생성물 1

HCID 100241891(6H)-Pyridazinenonanoic acid, 6-oxo-3,4-diphenyl-수율 69.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of methyl 6-oxo-3,4-diphenyl-1(6H)-pyridazinenonanoate (6 g, 14 mmol), 5N NaOH solution (8.6 mL, 43 mmol) and methanol (100 mL) was heated to reflux on a steam bath. After 30 minutes, the mixture was concentrated, diluted with water and acidified to pH=1 with 2N HCl solution. The mixture was extracted with CH2Cl2, the combined extracts dried over sodium sulfate and concentrated to leave an oil that crystallized on standing. Recrystallization from a mixture of CH2Cl2 and hexanes gave 6-oxo-3,4-diphenyl-1(6H)-pyridazinenonanoic acid (3.92 g, 67%) mp 100°-103° C.

후처리

  1. temperaturewas heated
  2. temperatureto reflux on a steam bath
  3. concentrationthe mixture was concentrated
  4. additiondiluted with water
  5. extractionThe mixture was extracted with CH2Cl2
  6. dry with materialthe combined extracts dried over sodium sulfate
  7. concentrationconcentrated
  8. customto leave an oil that
  9. customcrystallized
  10. customRecrystallization
  11. additionfrom a mixture of CH2Cl2 and hexanes

출처 및 근거

ORD 기록
ord-4ebc8029707b4a02b6aaca8aaaed7544
출처 데이터셋
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04992439

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