反应详情

Oxalyl chloride (0.6 mL, 6.9 mmol) was added dropwise to a solution of 2,4,6-triisopropylphenyl acetic acid (1.52 g, 5.8 mmol) in 150 mL toluene with 4 drops of N,N-dimethylformamide as a catalyst. The resulting solution was stirred overnight and then concentrated in vacuo. The residue was redissolved in 150 mL dichloromethane. Sulfamic acid 2,6-diisopropyl-4-thiocyanato-phenyl ester (1.70 g, 5.8 mmol) and triethylamine (2.0 mL) were added, and the resulting mixture was stirred for 2 hours. Washed with 1M HCl, dried the organic layer over magnesium sulfate, filtered, and concentrated to give 2.24 g of [(2,4,6-triisopropyl-phenyl)-acetyl]-sulfamic acid 2,6-diisopropyl-4-thiocyanato-phenyl ester as a white solid; mp 164-165° C.

1. concentrationconcentrated in vacuo
2. dissolutionThe residue was redissolved in 150 mL dichloromethane
3. stirringthe resulting mixture was stirred for 2 hours
4. washWashed with 1M HCl
5. dry with materialdried the organic layer over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated