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

HRID 1269809ノート

反応式

HRID 1269809 の反応式
[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

参加物

4

反応物 2

HCID 204431481,4-Dioxane hydrochlorideHCID 22933697HCID 22933697、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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%).

後処理

  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))

出典と根拠

ORDレコード
ord-d0b1fc5b89074ca7abb149cf92859a5f
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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