1,1'-Carbonyldiimidazole → 3,4-Dihydro-3-methyl-2(1H)-quinazolinone
반응식
[C:1]([N:8]1[CH:12]=[CH:11]N=[CH:9]1)([N:3]1[CH:7]=[CH:6]N=C1)=[O:2].CN[CH2:15][C:16]1C=CC=C[C:17]=1N>C1COCC1>[CH3:9][N:8]1[CH2:12][C:11]2[C:7](=[CH:6][CH:15]=[CH:16][CH:17]=2)[NH:3][C:1]1=[O:2]참가 물질
4
실험 절차
1,1'-Carbonyl-diimidazole (16.7 g) is added to a solution of 2-(methylaminomethyl)-aniline (11.2 g) in anhydrous THF (30 ml) under nitrogen. The reaction mixture is refluxed for about 24 hours, stirred for 48 hours at RT and filtered. The filtered precipitate is suspended in 2N HCl for about 40 minutes, filtered, and the filtered solid washed with water and air dried, affording the desired product, M.P. 202-206.5 C., used in the next step without further purification.
후처리
- temperatureThe reaction mixture is refluxed for about 24 hours
- filtrationfiltered
- waitThe filtered precipitate is suspended in 2N HCl for about 40 minutes
- filtrationfiltered
- washthe filtered solid washed with water and air
- customdried
출처 및 근거
- ORD 기록
- ord-fa30c02c503e45eda724856b9cdf3a4e
- 출처 데이터셋
- uspto-grants-1989_09
- 특허 번호
- US04868300
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