Sodium Hydroxide → HCID 178433897, 화합물

HRID 497950노트

반응식

HRID 497950 반응식
[OH:1][C:2]1[C:7](C(O)=O)=[CH:6][N:5]=[C:4]2[N:11]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=3)[N:12]=[C:13]([CH3:14])[C:3]=12.[OH-].[Na+]>P(=O)(O)(O)O>[CH3:14][C:13]1[C:3]2[C:2]([OH:1])=[CH:7][CH:6]=[N:5][C:4]=2[N:11]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][N:16]=2)[N:12]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 178433901HCID 178433901, 화합물

생성물 1

HCID 178433897HCID 178433897, 화합물수율 15.2%

시약·촉매·용매 1

HCID 1004Phosphoric Acid용매

반응 조건

온도
180 °C

실험 절차

A suspension of 4-hydroxy-3-methyl-1-(2-pyridinyl)-1H-pyrazolo[3,4-b]pyridine-5-carboxylic acid (2.0 g, 6.7 mmol) in phosphoric acid (10 mL) was heated and stirred at 180° C. for 12 hours. The reaction solution was cooled to room temperature, neutralized by the addition of an aqueous sodium hydroxide solution, and organic matter was extracted with chloroform. The extract was washed with saturated brine and water, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. Purification of the residue by silica gel column chromatography (chloroform:methanol=95:5) gave the title compound (230 mg, 15% yield).

후처리

  1. temperaturewas heated
  2. temperatureThe reaction solution was cooled to room temperature
  3. extractionwas extracted with chloroform
  4. washThe extract was washed with saturated brine and water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customPurification of the residue by silica gel column chromatography (chloroform:methanol=95:5)

출처 및 근거

ORD 기록
ord-6c8cf89897c141e495cb6985d2680b0e
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06949648B2

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