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

HRID 30403ノート

反応式

HRID 30403 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-90ee85a79c5f4fa7aa801a35fb58813c
出典データセット
uspto-grants-2008_09
特許番号
US07423054B2

反応ノート

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