反应详情

Trifluoroacetic acid (6 mL) was added to the product from step (x) (505 mg) and the mixture was stirred at RT for 14 h. After the reaction mixture was concentrated, 1M-sodium hydroxide (20 mL) and methanol (10 mL) was added to the residue and the mixture was stirred in methanol for 30 mins. The reaction mixture was concentrated, diluted with water and washed with chloroform. The aqueous layer was neutralized with 6M-hydrogen chloride and sat. sodium hydrogen dicarbonate and extracted with chloroform/EtOH (3/1). The combined organic layer was dried and concentrated. The residue was diluted with chloroform, filtered, concentrated and diluted with chloroform/EtOAc. The precipitate was collected by filtration, washed with EtOAc and dried to give 450 mg of the sub-title compound as a white solid; 1H NMR (CDCl3); 6.78 (1H, d), 6.48 (1H, d), 6.38 (1H, dd), 5.35-5.20 (1H, m), 4.20-3.97 (3H, m), 3.86 (3H, s), 3.55 (2H, s), 3.63-3.47 (1H, m), 3.40-3.09 (4H, m), 2.91-2.75 (1H, m), 2.60-2.45 (1H, m), 2.35 (3H, s), 2.30-2.02 (4H, m), 2.02-1.70 (3H, m), 1.50-1.33 (1H, m), 1.33-0.95 (5H, m), 0.77 (3H, t); LC-MS: m/z 516.

1. concentrationAfter the reaction mixture was concentrated
2. addition1M-sodium hydroxide (20 mL) and methanol (10 mL) was added to the residue
3. stirringthe mixture was stirred in methanol for 30 mins
4. concentrationThe reaction mixture was concentrated
5. additiondiluted with water
6. washwashed with chloroform
7. extractionextracted with chloroform/EtOH (3/1)
8. customThe combined organic layer was dried
9. concentrationconcentrated
10. additionThe residue was diluted with chloroform
11. filtrationfiltered
12. concentrationconcentrated
13. additiondiluted with chloroform/EtOAc
14. filtrationThe precipitate was collected by filtration
15. washwashed with EtOAc
16. customdried