反应详情

To a solution of the product of Step A (0.05 g; 0.143 mmol) in dioxane (1 ml) 2N KOH (0.36 ml; 0.72 mmol) was added and the mixture was refluxed for 15 min, cooled to room temperature and evaporated to dryness under reduced pressure. The residue was diluted to 2 ml with H2O and filtered. The filtrate was acidified to pH ˜4 with citric acid. The solid formed was filtered off, washed with H2O (3×2 ml), dried in vacuo to give the title compound (0.03 g; 65%), as a colourless solid. 1H-NMR (CD3OD+CDCl3) 7.16 (d, 2H, J=8.4 Hz); 7.0 (d, 2H, J=8.4 Hz); 4.21 (s, CD3OH); 3.4 (t, 2H, J=6.7 Hz); 2.73 (m, 4H); 2.5-2.44 (m, 4H); 1.5 (m, 2H); 1.2 (m, 10H); 0.81 (m, 3H).

1. temperaturethe mixture was refluxed for 15 min
2. customevaporated to dryness under reduced pressure
3. additionThe residue was diluted to 2 ml with H2O
4. filtrationfiltered
5. customThe solid formed
6. filtrationwas filtered off
7. washwashed with H2O (3×2 ml)
8. customdried in vacuo