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Sodium Hydroxide → [1-(6-Chloropyridazin-3-yl)-3-methyl-5-phenyl-1H-pyrazol-4-yl]acetic acid

HRID 2068482
ノート
印刷プレビュー

反応式

HRID 2068482 の反応式
[OH-].[Na+].C[O:4][C:5](=[O:26])[CH2:6][C:7]1[C:8]([CH3:25])=[N:9][N:10]([C:18]2[N:19]=[N:20][C:21]([Cl:24])=[CH:22][CH:23]=2)[C:11]=1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>CO>[Cl:24][C:21]1[N:20]=[N:19][C:18]([N:10]2[C:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[C:7]([CH2:6][C:5]([OH:26])=[O:4])[C:8]([CH3:25])=[N:9]2)=[CH:23][CH:22]=1
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

4

反応物 2

HCID 14798Sodium HydroxideHCID 131730043methyl[1-(6-chloropyridazin-3-yl)-3-methyl-5-phenyl-1H-pyrazol-4-yl]acetate

生成物 1

HCID 86642722[1-(6-Chloropyridazin-3-yl)-3-methyl-5-phenyl-1H-pyrazol-4-yl]acetic acid

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
20 °C

実験手順

0.058 g (1.444 mmol) of 2-molar aqueous sodium hydroxide solution was added to 0.099 g (0.289 mmol) of methyl[1-(6-chloropyridazin-3-yl)-3-methyl-5-phenyl-1H-pyrazol-4-yl]acetate in 5.00 ml of methanol, and the mixture was stirred at 20° C. for 1 h. The methanol was removed under reduced pressure and the residue was poured into a mixture of 10 ml of water and 15 ml of dichloromethane. The aqueous phase was extracted with 15 ml of dichloromethane, acidified with concentrated hydrochloric acid (pH=3) and extracted three times with in each case 15 ml of dichloromethane. Drying of the combined organic phases and removal of the solvent under reduced pressure gave 0.052 g (54.7% of theory) of a brown wax-like solid.

後処理

  1. customThe methanol was removed under reduced pressure
  2. additionthe residue was poured into a mixture of 10 ml of water and 15 ml of dichloromethane
  3. extractionThe aqueous phase was extracted with 15 ml of dichloromethane
  4. extractionextracted three times with in each case 15 ml of dichloromethane
  5. customDrying of the combined organic phases and removal of the solvent under reduced pressure
  6. customgave 0.052 g (54.7% of theory) of a brown wax-like solid

出典と根拠

ORDレコード
ord-d36ab2cede2943ae9d71b6046240b9b9
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08298994B2

反応ノート

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