반응식
Cl[CH2:2][C:3]1[C:4]([CH3:9])=[N:5][O:6][C:7]=1[CH3:8].[NH3:10]>>[NH2:10][CH2:2][C:3]1[C:4]([CH3:9])=[N:5][O:6][C:7]=1[CH3:8]참가 물질
3
실험 절차
4-Chloromethyl-3,5-dimethylisoxazole (700 mg, 4.8 mmol) is suspended in concentrated aqueous ammonia at 20-25 degrees C., and vigorously stirred overnight. The reaction mixture is extracted with isopropyl alcohol/chloroform (10/90, 2×). The combined organic phases are concentrated under nitrogen flow. The residue is purified by flash chromatography methanol/methylene chloride (5-20%, 1% triethylamine) to give the title compound, MR (CDCl3, 300 MHz) delta 3.62, 2.37, 2.29, and 1.44.
후처리
- customvigorously stirred overnight
- extractionThe reaction mixture is extracted with isopropyl alcohol/chloroform (10/90, 2×)
- concentrationThe combined organic phases are concentrated under nitrogen flow
- customThe residue is purified by flash chromatography methanol/methylene chloride (5-20%, 1% triethylamine)
출처 및 근거
- ORD 기록
- ord-baadfe228970474f9ccf855c160cc0da
- 출처 데이터셋
- uspto-grants-2009_03
- 특허 번호
- US07498436B2
연결된 노트
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