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Sodium Hydroxide → [3-Methyl-1-(4-methylpyridin-3-yl)-5-phenyl-1H-pyrazol-4-yl]acetic acid

HRID 888726
ノート
印刷プレビュー

反応式

HRID 888726 の反応式
[OH-].[Na+].[CH3:3][C:4]1[C:8]([CH2:9][C:10]([O:12]C)=[O:11])=[C:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:6]([C:20]2[CH:21]=[N:22][CH:23]=[CH:24][C:25]=2[CH3:26])[N:5]=1>CO>[CH3:3][C:4]1[C:8]([CH2:9][C:10]([OH:12])=[O:11])=[C:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[N:6]([C:20]2[CH:21]=[N:22][CH:23]=[CH:24][C:25]=2[CH3:26])[N:5]=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 86626934Methyl [3-methyl-1-(4-methylpyridin-3-yl)-5-phenyl-1H-pyrazol-4-yl]acetate

生成物 1

HCID 68818330[3-Methyl-1-(4-methylpyridin-3-yl)-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

0.100 g (2.489 mmol) of 2 molar aqueous sodium hydroxide solution was added to 0.200 g (0.498 mmol) of methyl [3-methyl-1-(4-methylpyridin-3-yl)-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 onto 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 give 0.108 g (71% of theory) of a yellow solid of melting point 246° C.

後処理

  1. customThe methanol was removed under reduced pressure
  2. additionthe residue was poured onto 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. customgive 0.108 g (71% of theory) of a yellow solid of melting point 246° C.

出典と根拠

ORDレコード
ord-a531c57b56a4410ca1282e9efbb24737
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08252723B2

反応ノート

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