Toluene → HCID 22933850、化合物

HRID 1269766ノート

反応式

HRID 1269766 の反応式
O1CCOCC1.[ClH:7].[NH:8]1[C:16]2[C:11](=[CH:12][C:13]([C:17]([NH:19][CH2:20][CH:21]3[CH2:26][CH2:25][N:24](C(OC(C)(C)C)=O)[CH2:23][CH2:22]3)=[O:18])=[CH:14][CH:15]=2)[CH:10]=[N:9]1.C1(C)C=CC=CC=1>O1CCOCC1.C(O)(=O)C>[ClH:7].[NH:24]1[CH2:25][CH2:26][CH:21]([CH2:20][NH:19][C:17]([C:13]2[CH:12]=[C:11]3[C:16](=[CH:15][CH:14]=2)[NH:8][N:9]=[CH:10]3)=[O:18])[CH2:22][CH2:23]1

参加物

6

反応物 3

HCID 1140TolueneHCID 184475431,1-Dimethylethyl 4-[[(1H-indazol-5-ylcarbonyl)amino]methyl]-1-piperidinecarboxylateHCID 204431481,4-Dioxane hydrochloride

生成物 1

HCID 22933850HCID 22933850、化合物収率 101.1%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

A 4N-hydrogen chloride-1,4-dioxane solution (0.200 mg, 0.800 mmol) was added to a solution of tert-butyl 4-{[(1H-indazol-5-ylcarbonyl)amino]methyl}piperidine-1-carboxylate (36.0 mg, 0.100 mmol) in a mixture of 1,4-dioxane (0.4 ml) and acetic acid (0.7 ml) at room temperature, and the resulting mixture was stirred for 3 hours while being maintained at room temperature. Toluene was added to the reaction solution and the resulting mixture was stirred while being maintained at room temperature. Then, the resulting slurry was collected by filtration and dried under reduced pressure, and the resulting crude product residue was stirred in methanol (3.0 ml) for 1 hour with heating under reflux while maintaining the temperature. The resulting mixture was concentrated to dryness to obtain N-(piperidin-4-ylmethyl)-1H-indazole-5-carboxamide hydrochloride (29.8 mg, 100%).

後処理

  1. stirringthe resulting mixture was stirred
  2. temperaturewhile being maintained at room temperature
  3. filtrationThen, the resulting slurry was collected by filtration
  4. customdried under reduced pressure
  5. stirringthe resulting crude product residue was stirred in methanol (3.0 ml) for 1 hour
  6. temperaturewith heating
  7. temperatureunder reflux
  8. temperaturewhile maintaining the temperature
  9. concentrationThe resulting mixture was concentrated to dryness

出典と根拠

ORDレコード
ord-3aee8ef091314cd880c46e3be61a6b87
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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