Sodium Bicarbonate → N-(1H-indazol-5-ylmethyl)-4-piperidinecarboxamide

HRID 1269736ノート

反応式

HRID 1269736 の反応式
Cl.O1CCOCC1.[NH:8]1[C:16]2[C:11](=[CH:12][C:13]([CH2:17][NH:18][C:19]([CH:21]3[CH2:26][CH2:25][N:24](C(OC(C)(C)C)=O)[CH2:23][CH2:22]3)=[O:20])=[CH:14][CH:15]=2)[CH:10]=[N:9]1.C(=O)([O-])O.[Na+]>>[NH:8]1[C:16]2[C:11](=[CH:12][C:13]([CH2:17][NH:18][C:19]([CH:21]3[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]3)=[O:20])=[CH:14][CH:15]=2)[CH:10]=[N:9]1

参加物

4

反応物 3

HCID 516892Sodium BicarbonateHCID 18447544tert-butyl 4{[(1H-indazol-5-ylmethyl)amino]carbonyl}-1-piperidinecarboxylateHCID 204431481,4-Dioxane hydrochloride

生成物 1

HCID 22933995N-(1H-indazol-5-ylmethyl)-4-piperidinecarboxamide収率 9%

実験手順

A 4N-hydrochloric acid/dioxane solution (2.0 ml) was added to tert-butyl 4{[(1H-indazol-5-ylmethyl)amino]carbonyl}-1-piperidinecarboxylate (160 mg, 0.446 mmol), and the resulting mixture was stirred at room temperature for 2 hours. Then, the reaction solution was poured into a saturated aqueous sodium hydrogencarbonate solution and extracted with chloroform. The organic layer was dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent. The resulting residue was recrystallized from a mixture of ethanol and diethyl ether to obtain N-(1H-indazol-5-ylmethyl)-4-piperidinecarboxamide (10 mg, 9%).

後処理

  1. extractionextracted with chloroform
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. distillationdistilled under reduced pressure
  4. customto remove the solvent
  5. customThe resulting residue was recrystallized from a mixture of ethanol and diethyl ether

出典と根拠

ORDレコード
ord-329f523df6794833a2fe812bb7dfd37e
出典データセット
uspto-grants-2007_04
特許番号
US07199147B2

反応ノート

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