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

HRID 1912924노트

반응식

HRID 1912924 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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)+.

후처리

  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)

출처 및 근거

ORD 기록
ord-ebe9207079224b71ab60b3c661079019
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609669B2

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