Hydrochloric Acid → 1-butyl-1H-indazole-6-carboxylic acid

HRID 14165

反応式

HRID 14165 の反応式
[CH2:1]([N:5]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([C:14]([O:16]C)=[O:15])[CH:12]=2)[CH:7]=[N:6]1)[CH2:2][CH2:3][CH3:4].C(=O)(O)[O-].[Na+].[OH-].[Na+].Cl>CO>[CH2:1]([N:5]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([C:14]([OH:16])=[O:15])[CH:12]=2)[CH:7]=[N:6]1)[CH2:2][CH2:3][CH3:4]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 21086132Methyl 1-butyl-1H-indazole-6-carboxylate

生成物 1

HCID 210851661-butyl-1H-indazole-6-carboxylic acid収率 92.7%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
80 °C

実験手順

To a mixture of methyl 1-butyl-1H-indazole-6-carboxylate (0.356 g) in methanol (10 mL) was added saturated sodium bicarbonate (5 mL). The mixture was heated at 60° C. for 2 h at which time 1N NaOH (5 mL) was added and the mixture heated to 80° C. for 18 h. The mixture was cooled to room temperature, poured into 1N HCl (50 mL), and extracted with ethyl acetate. The ethyl acetate extract dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give 0.310 g of the title compound: 1H NMR (CDCl3) δ 0.964, 1.96, 4.48, 7.81, 7.89, 8.29, 8.46.

後処理

  1. additionwas added
  2. temperatureThe mixture was cooled to room temperature
  3. extractionextracted with ethyl acetate
  4. extractionThe ethyl acetate extract
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-b16ed85681fb4419a9f9e0e322cad156
出典データセット
uspto-grants-2010_06
特許番号
US07727997B2

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