반응식
Cl[C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[C:4]([O:14][C:15]2[CH:16]=[C:17]([CH:20]=[CH:21][C:22]=2[O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:18]#[N:19])[CH:3]=1.C([O-])([O-])=O.[Cs+].[Cs+].[OH:37][C:38]1[CH:39]=[C:40]([C:44]2[N:45]([CH3:49])[CH2:46][CH2:47][N:48]=2)[CH:41]=[CH:42][CH:43]=1>CS(C)=O>[CH3:49][N:45]1[CH2:46][CH2:47][N:48]=[C:44]1[C:40]1[CH:39]=[C:38]([CH:43]=[CH:42][CH:41]=1)[O:37][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[C:4]([O:14][C:15]2[CH:16]=[C:17]([CH:20]=[CH:21][C:22]=2[O:23][CH2:24][C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:18]#[N:19])[CH:3]=1참가 물질
5
반응물 3
생성물 1
시약·촉매·용매 1
반응 조건
- 온도
- 50 °C
실험 절차
To 3-[(6-chloro-2-phenylpyrimidin-4-yl)oxy]-4-(benzyloxy)benzonitrile (1.0 g, 2.4 mmol) in DMSO (12 mL) was added Cs2CO3 (0.8 g, 2.5 mmol) and 2-(3-hydroxyphenyl)-1-methylimidazoline (0.44 g, 2.5 mmol). After stirring in an oil bath at 50° C. for 24 hours, the reaction was partitioned with water and ethyl acetate. The layers were separated, washed with water and brine, dried (Na2SO4), and the solvent was removed in vacuo. The residue was chromatographed on silica gel with CH2CL2 /MeOH/NH4OH (120/5/1) to give 0.5 g of 3-[(6-[3-(1-methylimidazolin-2-yl)phenoxy]-2-phenylpyrimidin-4-yl)oxy]-4-(benzyloxy)benzonitrile.
후처리
- customthe reaction was partitioned with water and ethyl acetate
- customThe layers were separated
- washwashed with water and brine
- dry with materialdried (Na2SO4)
- customthe solvent was removed in vacuo
- customThe residue was chromatographed on silica gel with CH2CL2 /MeOH/NH4OH (120/5/1)
출처 및 근거
- ORD 기록
- ord-323eb7ecb9dd4b0bb68bc1e565b34d4d
- 출처 데이터셋
- uspto-grants-2000_10
- 특허 번호
- US06127376
연결된 노트
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