Sodium Hydroxide → 1-((4-methoxyphenyl)methyl)-1H-indazole-3-carboxylic acid

HRID 1372789

反応式

HRID 1372789 の反応式
[CH3:1][O:2][C:3]1[CH:22]=[CH:21][C:6]([CH2:7][N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]([C:17]([O:19]C)=[O:18])=[N:9]2)=[CH:5][CH:4]=1.[OH-].[Na+]>C1COCC1.Cl>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][C:6]([CH2:7][N:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[C:10]([C:17]([OH:19])=[O:18])=[N:9]2)=[CH:21][CH:22]=1

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 17859014methyl 1-((4-methoxyphenyl)methyl)-1H-indazole-3-carboxylate

生成物 1

HCID 178594441-((4-methoxyphenyl)methyl)-1H-indazole-3-carboxylic acid収率 80%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

Methyl 1-(4-methoxybenzyl)-3-indazolylcarboxylate (830 mg, 2.80 mmol) was dissolved in THF (22 ml). To the resulting solution was added 0.25N NaOH (22 ml, 5.60 mmol). The resulting mixture was stirred for 15 hours at room temperature. The reaction mixture was poured in 1N HCl (50 ml), followed by extraction with chloroform (2×100 ml). The extract was dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The residue was dissolved in chloroform and hexane was added to the resulting solution until precipitation appeared. The crystals thus precipitated were collected by filtration under reduced pressure and dried for 12 hours under reduced pressure to give 1-(4-methoxybenzyl)-3-indazolylcarboxylicacid (630 mg, 80%) as a colorless amorphous substance.

後処理

  1. extractionfollowed by extraction with chloroform (2×100 ml)
  2. dry with materialThe extract was dried over anhydrous magnesium sulfate
  3. distillationdistilled under reduced pressure
  4. customto remove the solvent
  5. dissolutionThe residue was dissolved in chloroform
  6. additionhexane was added to the resulting solution until precipitation
  7. customThe crystals thus precipitated
  8. filtrationwere collected by filtration under reduced pressure
  9. customdried for 12 hours under reduced pressure

出典と根拠

ORDレコード
ord-44fa06e71e484ca382967f1ba947822e
出典データセット
uspto-grants-2007_01
特許番号
US07157487B2

関連ノート

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