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

HRID 981475
ノート
印刷プレビュー

反応式

HRID 981475 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4ebc8029707b4a02b6aaca8aaaed7544
出典データセット
uspto-grants-1991_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04992439

反応ノート

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