反应详情

To a solution of 3 (3.6 g, 8.54 mmol) in THF (21 mL) was added portionwise aqueous 4 M HCl at 0° C. The mixture was allowed to reach room temperature and stirred over 5 h. A white precipitated that formed during the reaction was filtered and washed with THF. Two recrystallizations affored 4 (2.88 g, 91.2%) as a white solid. 1H NMR (400 MHz, DMSO) ä 11.30 (s, 1H), 8.62 (br s, 3H), 7.46-7.15 (m, 5H), 4.97 (m, 2H), 3.59 (m, 2H), 2.98 (m, 2H), 2.76 (m, 1H), 2.58 (m, 1H), 2.24-1.97 (m, 2H), 1.85 (m, 2H), 1.74 (m, 1H), 1.21 (m, 1H).

1. customto reach room temperature
2. customA white precipitated
3. customthat formed during the reaction
4. filtrationwas filtered
5. washwashed with THF
6. customTwo recrystallizations