反应详情

A solution of 2-chloro-N-(1,1-dimethylethyl)-6-phenylbenzenesulfonamide (23 g, 0.071 mol) in a mixture of 120 ml trifluoroacetic acid (TFA) plus 4 ml water was heated to reflux for 2 hours. The TFA was evaporated in vacuo and the residue partitioned between methylene chloride and water. The organic layer was dried (MgSO4), evaporated, and the residue crystallized from ether/methylene chloride to afford 15.9 g of crystalline solid in two crops, m.p. 185°-87°. NMR (90 MHZ, CDCl3) 6.45 (s, br, NH2). 7.3-7.7 (m, 8H) ppm.

1. temperaturewas heated
2. temperatureto reflux for 2 hours
3. customThe TFA was evaporated in vacuo
4. customthe residue partitioned between methylene chloride and water
5. dry with materialThe organic layer was dried (MgSO4)
6. customevaporated
7. customthe residue crystallized from ether/methylene chloride