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1-Bromopropane → 1-Propyl-1h-indazole-3-carboxylic acid

HRID 1586452
ノート
印刷プレビュー

反応式

HRID 1586452 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([C:10]([OH:12])=[O:11])=[N:2]1.[H-].[Na+].Br[CH2:16][CH2:17][CH3:18]>CN(C=O)C>[CH2:16]([N:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([C:10]([OH:12])=[O:11])=[N:2]1)[CH2:17][CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 78401-BromopropaneHCID 24758Sodium hydrideHCID 78250Indazole-3-carboxylic acid

生成物 1

HCID 106320111-Propyl-1h-indazole-3-carboxylic acid収率 67.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1H-indazole-3-carboxylic acid (5.00 g) in DMF (40 ml) was gradually added 60% sodium hydride (1.55 g) at 0° C. with stirring, and the mixture was stirred at room temperature for one hour. Then 1-bromopropane (4.55 g) was added, and the mixture was stirred overnight. The reaction solution was distilled off, dissolved in water, and washed with ethyl acetate. The aqueous layer was made acidic with hydrochloric acid, extracted with ethyl acetate, then the extract was dried over anhydrous magnesium sulfate, and decolorized with active carbon. After the solvent was distilled off, crystallization from ether gave the title compound (4.24 g) as crystals. Yield=67%.

後処理

  1. customat 0° C.
  2. stirringthe mixture was stirred at room temperature for one hour
  3. stirringthe mixture was stirred overnight
  4. distillationThe reaction solution was distilled off
  5. dissolutiondissolved in water
  6. washwashed with ethyl acetate
  7. extractionextracted with ethyl acetate
  8. dry with materialthe extract was dried over anhydrous magnesium sulfate
  9. distillationAfter the solvent was distilled off
  10. customcrystallization from ether

出典と根拠

ORDレコード
ord-738ee3fc61c6471c95a8397993440009
出典データセット
uspto-grants-1999_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05945434

反応ノート

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