反应详情

Bezenesulfonic acid monohydrate (1.06 g, 6 mmol) was dried by azeotroping off the water of a benzene solution (twice) and adding the dried acid solution to a solution of example 415 (2.81 g, 6 mmol) in toluene (40 ml). The solvents were removed in vacuo (twice) and the resulting residue recrystallized twice from toluene and dried under high vacuum overnight give 2.77 g of benzenesulfonic acid salt as a white solid. mp 157-159° C. [α]D25=+16.9° (CH3OH, c=0.23 g/dL). Anal. Calcd for C34H42N3O5FS: C, 65.47; H, 6.80; N, 6.75; S, 5.14. Found: C, 65.48; H, 6.80; N, 6.70; S, 5.35.

1. customby azeotroping off the water of a benzene solution (twice) and
2. customThe solvents were removed in vacuo (twice) and the resulting residue
3. customrecrystallized twice from toluene
4. customdried under high vacuum overnight