Triethylamine → HCID 68849595、化合物
反応式
[I:1][C:2]1[CH:3]=[N:4][C:5]([N:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[N:6][CH:7]=1.C(N(CC)CC)C.[CH3:21][S:22](Cl)(=[O:24])=[O:23]>ClCCl>[I:1][C:2]1[CH:3]=[N:4][C:5]([N:8]2[CH2:9][CH2:10][N:11]([S:22]([CH3:21])(=[O:24])=[O:23])[CH2:12][CH2:13]2)=[N:6][CH:7]=1参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a stirred solution of 5-iodo-2-piperazin-1-ylpyrimidine (7.0 g, 24.1 mmol, CAS number 95847-41-9) and triethylamine (10 mL, 72 mmol) in dichloromethane (70 mL) at 0° C. was added methanesulfonyl chloride (1.93 mL, 138 mmol) dropwise over 10 minutes. The reaction was then stirred for 30 minutes at 0° C., before being allowed to warm to room temperature and stirred for an additional 30 minutes. The reaction was then quenched with water (70 mL) and the layers were separated. The organic phase was washed with water (100 mL) and the organics were dried (MgSO4), filtered and evaporated in vacuo. The residue was then triturated with ethyl acetate and the solid residue filtered and dried in vacuo to give 5-iodo-2-[4-(methylsulfonyl)piperazin-1-yl]pyrimidine as an off white solid (8.85 g, 24 mmol, 99%).