Dimethylformamide dimethyl acetal → 4-Methyl-2-(methylsulfanyl)pyrimidine
반응식
[SH:1][C:2]1[N:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N:3]=1.Cl.[CH:10](N(C(C)C)CC)(C)C.COC(OC)N(C)C>C1(C)C=CC=CC=1>[CH3:10][S:1][C:2]1[N:7]=[C:6]([CH3:8])[CH:5]=[CH:4][N:3]=1참가 물질
5
실험 절차
To 2-mercapto-4-methylpyrimidine·HCl (50.0 g, 0.307 mole) in toluene (750 mL), under argon, was added diisopropylethylamine (80.0 mL, 0.461 mole) followed by N,N-dimethylformamide dimethyl acetal (100 mL) and the mixture heated to reflux for 4 hours. Upon cooling, the reaction was concentrated in vacuo to an oil, dissolved in ether (400 mL), and washed with water (2×50 mL). The organic extract was dried over anhydrous sodium sulfate, filtered and concentrated to an oil which was vacuum distilled to give 2-methylthio-4-methylpyrimidine (36.4 g) as an oil.
후처리
- temperaturethe mixture heated
- temperatureto reflux for 4 hours
- temperatureUpon cooling
- concentrationthe reaction was concentrated in vacuo to an oil
- dissolutiondissolved in ether (400 mL)
- washwashed with water (2×50 mL)
- extractionThe organic extract
- dry with materialwas dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated to an oil which
- distillationdistilled
출처 및 근거
- ORD 기록
- ord-a19ceaf028184881a3776d4a7655c208
- 출처 데이터셋
- uspto-grants-1999_01
- 특허 번호
- US05859041
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