反应详情

温度

0 °C

To a solution of 2-mesitylene sulphonyl chloride (2.0 g, 9.14 mmol) in dry THF (50 mL), was added N-Boc-hydroxylamine (1.21 g, 9.14 mmol) and cooled to 0° C. under N2 atmosphere. The reaction mixture was stirred for 5 minutes. To this mixture triethylamine (1.1 g, 11 mmol) was added slowly over 10 minutes. The reaction mixture was stirred for 1 hour at 0° C. and upon completion, the solvent removed in vacuo. The residue was redissolved in dichloromethane (50 mL) and washed with water (2×50 mL), 10% aqueous NaHCO3 (50 mL) and dried over MgSO4. It was then concentrated under reduced pressure at room temperature to get the product as an off white solid; (2.1 g, 73%). TLC: pet ether/ethyl acetate (8/2) Rf-0.4. 1H NMR (DMSO-d6; 400 MHz): δ 11.16 (s, 1H), 7.12 (s, 2H), 2.49 (s, 6H), 2.28 (s, 3H), 1.23 (s, 9H).

1. stirringThe reaction mixture was stirred for 1 hour at 0° C. and upon completion
2. customthe solvent removed in vacuo
3. dissolutionThe residue was redissolved in dichloromethane (50 mL)
4. washwashed with water (2×50 mL), 10% aqueous NaHCO3 (50 mL)
5. dry with materialdried over MgSO4
6. concentrationIt was then concentrated under reduced pressure at room temperature
7. customto get the product as an off white solid