反应详情

A solution of 480 mg of 19b in 10 ml of dioxane was mixed with 200 mg of KOH in 2 ml of water. The mixture was stirred at rt for 3 h and then diluted with 40 ml of water and acidified to pH 3 with 0.5 N HCl. The product was extracted with ethyl acetate. The organic layer was washed with water, dried and concentrated, to provide 420 mg of 19c as white amorphous material; MS-ESI: [M+1] 495.19 and 493.18. NMR (CDCl3) δ 1.43 (m, 2, CH2), 1.53 (s, 9, tertC4H9), 1.68-1.90 (bm, 2, CH2), 1.92 (t, 1, CH), 2.16 (m, 2, CH2), 2.80-3.00 (bm, 2, CH2), 3.22-3.45 (bm, 2, CH2), 3.68 (m, 2, CH2), 3.88 (s, 3, OCH3), 5.74 (s, 1, CH), 6.65 (s, 1, ArH), 7.73 (s, 1, ArH).

1. extractionThe product was extracted with ethyl acetate
2. washThe organic layer was washed with water
3. customdried
4. concentrationconcentrated