Methanol → 4-(2,5-dimethylpyrimidin-4-yl)-1-methyl-1H-pyrazole-5-carboxylic acid

HRID 60137ノート

反応式

HRID 60137 の反応式
[OH-].[Na+].CO.[CH3:5][C:6]1[N:11]=[C:10]([C:12]2[CH:13]=[N:14][N:15]([CH3:21])[C:16]=2[C:17]([O:19]C)=[O:18])[C:9]([CH3:22])=[CH:8][N:7]=1>O>[CH3:5][C:6]1[N:11]=[C:10]([C:12]2[CH:13]=[N:14][N:15]([CH3:21])[C:16]=2[C:17]([OH:19])=[O:18])[C:9]([CH3:22])=[CH:8][N:7]=1

参加物

5

反応物 3

HCID 887MethanolHCID 14798Sodium HydroxideHCID 90383435methyl 4-(2,5-dimethylpyrimidin-4-yl)-1-methyl-1H-pyrazole-5-carboxylate

生成物 1

HCID 903834284-(2,5-dimethylpyrimidin-4-yl)-1-methyl-1H-pyrazole-5-carboxylic acid収率 52.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

Sodium hydroxide (0.31 g) was added to a mixed solution of methanol (15 ml) and water (15 ml) containing the methyl 4-(2,5-dimethylpyrimidin-4-yl)-1-methyl-1H-pyrazole-5-carboxylate (1.9 g) obtained in (Example 3.22) <Step 1>, and the obtained mixture was then stirred at 50° C. for 1 hour. Thereafter, methanol was distilled away from the reaction solution under reduced pressure, and the residue was then adjusted to pH 5-6 by addition of 1 N hydrochloric acid. Thereafter, water was distilled away under reduced pressure. The obtained residue was washed with methylene chloride, and the filtrate was then concentrated under reduced pressure, so as to obtain the title compound (0.94 g) in the form of a yellow solid.

後処理

  1. customobtained in (Example 3.22) <Step 1>
  2. distillationThereafter, methanol was distilled away from the reaction solution under reduced pressure
  3. additionthe residue was then adjusted to pH 5-6 by addition of 1 N hydrochloric acid
  4. distillationThereafter, water was distilled away under reduced pressure
  5. washThe obtained residue was washed with methylene chloride
  6. concentrationthe filtrate was then concentrated under reduced pressure

出典と根拠

ORDレコード
ord-00ee4882908340e589afcf098e444dae
出典データセット
uspto-grants-2016_09
特許番号
US09440970B2

反応ノート

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