反应详情

Combine hydrochloric acid (1.0M aq., 20 mL) with a solution of 6-(3,3-dimethyl-1,5-dioxa-spiro[5.5]undec-9-yloxy)-nicotinonitrile (2000 mg, 6.61 mmol) in acetone (25 mL). Stir at room temperature for 2 h then at 40–50° C. for 1 h. Concentrate the reaction mixture. Partition the residue between EtOAc/hex (25 mL) and K2CO3 (aq. sat. 20 mL). Wash the organic layer with water, brine, and dry it over sodium sulfate, filter and concentrate. Triturate the residue with EtOAc/hexanes (1/4) to provide a white solid which is further purified by flash chromatography (EtOAc/Hexanes 1/4) to give 1010 mg (71% yield) as a white solid.

1. waitat 40–50° C. for 1 h
2. concentrationConcentrate the reaction mixture
3. customPartition the residue between EtOAc/hex (25 mL) and K2CO3 (aq. sat. 20 mL)
4. washWash the organic layer with water, brine
5. dry with materialdry it over sodium sulfate
6. filtrationfilter
7. concentrationconcentrate
8. customTriturate the residue with EtOAc/hexanes (1/4)
9. customto provide a white solid which
10. customis further purified by flash chromatography (EtOAc/Hexanes 1/4)
11. customto give 1010 mg (71% yield) as a white solid