1,4-Dioxane hydrochloride → 5-[(Piperidin-3-yl)oxy]-1H-indazole

HRID 1269809노트

반응식

HRID 1269809 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([O:10][CH:11]3[CH2:16][CH2:15][CH2:14][N:13](C(OC(C)(C)C)=O)[CH2:12]3)=[CH:7][CH:8]=2)[CH:3]=[N:2]1.Cl.O1CCOCC1>CO>[NH:13]1[CH2:14][CH2:15][CH2:16][CH:11]([O:10][C:6]2[CH:5]=[C:4]3[C:9](=[CH:8][CH:7]=2)[NH:1][N:2]=[CH:3]3)[CH2:12]1

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 22933697HCID 22933697, 화합물

생성물 1

HCID 229334705-[(Piperidin-3-yl)oxy]-1H-indazole수율 101.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of the tert-butyl 3-(1H-indazol-5-yloxy)piperidine-1-carboxylate (150 mg, 0.473 mmol) obtained in Example 376 in methanol (2 ml) was added a 4N-hydrochloric acid-dioxane solution (1 ml) at room temperature. After 3 hours, the mixture thus obtained was concentrated under reduced pressure, and the resulting residue was dissolved in methanol. The resulting solution was adjusted to pH 8 to 9 with a 2M-aqueous sodium hydroxide solution and concentrated under reduced pressure. The residue was purified by a silica gel column chromatography (eluent: chloroform/methanol/chloroform/methanol/(1%-aqueous ammonia)) to obtain 5-(piperidin-3-yloxy)-1H-indazole (104 mg, 65%).

후처리

  1. customthe mixture thus obtained
  2. concentrationwas concentrated under reduced pressure
  3. dissolutionthe resulting residue was dissolved in methanol
  4. concentrationconcentrated under reduced pressure
  5. customThe residue was purified by a silica gel column chromatography (eluent: chloroform/methanol/chloroform/methanol/(1%-aqueous ammonia))

출처 및 근거

ORD 기록
ord-d0b1fc5b89074ca7abb149cf92859a5f
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199147B2

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