Acetylacetone → 3-Isopropyl-5,7-dimethylpyrazolo[1,5-a]pyrimidin-2-amine

HRID 1912924ノート

反応式

HRID 1912924 の反応式
[C:1]([CH2:4][C:5](=O)[CH3:6])(=O)[CH3:2].[CH:8]([C:11]1[C:12]([NH2:17])=[N:13][NH:14][C:15]=1[NH2:16])([CH3:10])[CH3:9].Cl.NO>C(O)(=O)C>[CH:8]([C:11]1[C:15]([NH2:16])=[N:14][N:13]2[C:1]([CH3:2])=[CH:4][C:5]([CH3:6])=[N:17][C:12]=12)([CH3:10])[CH3:9]

参加物

5

反応物 3

HCID 31261AcetylacetoneHCID 443297Hydroxyamine hydrochlorideHCID 687569004-Isopropyl-1H-pyrazole-3,5-diamine

生成物 1

HCID 687489893-Isopropyl-5,7-dimethylpyrazolo[1,5-a]pyrimidin-2-amine

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of acetylacetone (1034 mg, 10.33 mmol) and the product from Example 112B (965 mg, 6.88 mmol) in acetic acid (5 mL) was heated at 115° C. for 90 minutes, and then cooled to room temperature. Hydroxylamine hydrochloride (520 mg) was added, and the solution was stirred at room temperature for 14 hours, and then concentrated under vacuum. The residue was purified by HPLC (30×100 mm XBridge column eluted with 0.1 M aqueous (NH4)2CO3-MeOH, 60:40-0:100 over 15 min) to provide the title compound. MS (DCI/NH3) m/z 205 (M+H)+.

後処理

  1. concentrationconcentrated under vacuum
  2. customThe residue was purified by HPLC (30×100 mm XBridge column eluted with 0.1 M aqueous (NH4)2CO3-MeOH, 60:40-0:100 over 15 min)

出典と根拠

ORDレコード
ord-ebe9207079224b71ab60b3c661079019
出典データセット
uspto-grants-2013_12
特許番号
US08609669B2

反応ノート

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