Hydrochloric Acid → 1-(4-chloro-phenyl)-3-(piperidin-4-yloxy)-1H-indazole hydrochloride

HRID 30403노트

반응식

HRID 30403 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[C:23]3[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=3)[N:17]([C:24]3[CH:29]=[CH:28][C:27]([Cl:30])=[CH:26][CH:25]=3)[N:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.Cl.O1CCOCC1>CCOC(C)=O>[ClH:30].[Cl:30][C:27]1[CH:28]=[CH:29][C:24]([N:17]2[C:18]3[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:15]([O:14][CH:11]3[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]3)=[N:16]2)=[CH:25][CH:26]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 685301764-[1-(4-chloro-phenyl)-1H-indazol-3-yloxy]-piperidine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 574205501-(4-chloro-phenyl)-3-(piperidin-4-yloxy)-1H-indazole hydrochloride수율 171.9%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Intermediate 42 (212 mg, 0.495 mmol) was dissolved in EtOAc (2 ml), treated with 4M HCl in dioxane (1.61 ml, 6.44 mmol) and stirred overnight at room temperature. The mixture was concentrated in vacuo, treated with EtOAc and concentrated again. This process was repeated 5 times. The resulting white solid was triturated with Et2O, filtered, rinsed with Et2O and dried in a vacuum oven at 50° C. to afford 155 mg (86%) of the title product—1-(4-chloro-phenyl)-3-(piperidin-4-yloxy)-1H-indazole hydrochloride as a white solid.

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. additiontreated with EtOAc
  3. concentrationconcentrated again
  4. customThe resulting white solid was triturated with Et2O
  5. filtrationfiltered
  6. washrinsed with Et2O
  7. customdried in a vacuum oven at 50° C.

출처 및 근거

ORD 기록
ord-90ee85a79c5f4fa7aa801a35fb58813c
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423054B2

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