Toluene → HCID 22933850, 화합물

HRID 1269766노트

반응식

HRID 1269766 반응식
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

참가 물질

6

반응물 3

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

생성물 1

HCID 22933850HCID 22933850, 화합물수율 101.1%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 312751,4-Dioxane용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-3aee8ef091314cd880c46e3be61a6b87
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199147B2

반응 노트

불러오는 중…