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

HRID 60137노트

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HRID 60137 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

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온도
50 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-00ee4882908340e589afcf098e444dae
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440970B2

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