Sodium Hydroxide → HCID 178433897、化合物

HRID 497950ノート

反応式

HRID 497950 の反応式
[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

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 178433901HCID 178433901、化合物

生成物 1

HCID 178433897HCID 178433897、化合物収率 15.2%

試薬・触媒・溶媒 1

HCID 1004Phosphoric Acid溶媒

反応条件

温度
180 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-6c8cf89897c141e495cb6985d2680b0e
出典データセット
uspto-grants-2005_09
特許番号
US06949648B2

反応ノート

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