反应详情

温度

20 °C

To a solution of (2,4-dimethylphenyl)(2-methylpropyl)amine (300 mg, 1.692 mmol) in pyridine (5 mL), stirred in air at room temperature, was added 4-acetylbenzene-1-sulfonyl chloride (370 mg, 1.692 mmol) in one charge. The reaction mixture was stirred at 20° C. for 30 minutes, then left to stand overnight. The solvent was evaporated in vacuo then redissolved in methanol and passed through an aminopropyl (NH2) SPE cartridge, eluting with methanol, followed by 2M ammonia/methanol. The product containing fractions were combined and passed through a sulphonic acid (SCX) SPE cartridge eluting with methanol, followed by 2M ammonia/methanol. The product containing fractions were combined and evaporated under a stream of nitrogen to give the crude product. The crude was purified by flash (Si) chromatography (using a 0-50% ethyl acetate-cyclohexane gradient) to give the required product (282 mg) as a yellow gum. LCMS (M+1) 360, RT 1.35 mins.

1. additioncharge
2. waitleft
3. waitto stand overnight
4. customThe solvent was evaporated in vacuo
5. dissolutionthen redissolved in methanol
6. washeluting with methanol
7. additionThe product containing fractions
8. washeluting with methanol
9. additionThe product containing fractions
10. customevaporated under a stream of nitrogen
11. customto give the crude product
12. customThe crude was purified by flash (Si) chromatography (