反应详情

5.6 G. methyl-10,11-dihydrodibenzo[b,f]-thiepin-3-carboxylate is refluxed in a mixture of 50 cc. 20% aqueous sodium hydroxide and 50 cc. ethanol until a clear solution results (15 to 20 minutes). Most of the ethanol is evaporated away and aqueous residue is diluted with water and acidified with hydrochloric acid. The white solid is collected, recrystallized from acetic acid to yield 4.125 g. (77.7%) of the desired white crystalline material, m.p. 196°-198° C. Calculated: C: 70.29; H: 4.72; S: 12.51. Found: C: 69.92; H: 4.71; S: 12.15.

1. customMost of the ethanol is evaporated away
2. additionaqueous residue is diluted with water
3. customThe white solid is collected
4. customrecrystallized from acetic acid
5. customto yield 4.125 g