反应详情

7-Bromoindane-5-carboxylic acid (2.9 g, 12 mmol) and oxalylchloride (2.0 g, 16 mmol) were mixed with CH2Cl2 (50 mL) whereupon DMF (100 mg) was added. After 1 h at room temperature the mixture was poured into a mixture of concentrated NH4OH aq (20 mL) and ethanol (100 mL). The volatiles were removed by evaporation and the residue partitioned between ethyl acetate (100 mL) and water (50 mL). The organic layer was washed with brine and then dried over Na2SO4. The solvent was removed by evaporation and the solid residue was treated with cold CH2Cl2, then filtered off and dried. There was obtained 2.0 g (68%) of 7-bromoindane-5-carboxamide as a solid material. 1H NMR (300 MHz, CD3CO CD3): 2.0-2.2 (m, 2H), 2.8-2.9 (d, 2H), 2.9-3.0 (t, 1H), 3.0-3.1 (t, 1H), 6.5 (b, 1H), 7.4 (b, 1H), 7.7 (s, 1H), 7.9 (s,1H).

1. additionwas added
2. customThe volatiles were removed by evaporation
3. customthe residue partitioned between ethyl acetate (100 mL) and water (50 mL)
4. washThe organic layer was washed with brine
5. dry with materialdried over Na2SO4
6. customThe solvent was removed by evaporation
7. additionthe solid residue was treated with cold CH2Cl2
8. filtrationfiltered off
9. customdried