反应详情

(D)-Tartrate (10): To a 50 mL round bottom flask was added 1.63 g (5.53 mmol) of (R)-fluoxetine free amine (9). To this was added 20 mL of methanol and the amine was dissolved. To this solution was added 840 mg of (D)-tartaric acid (5.6 mmol). The reaction mixture was stirred for 30 minutes and then methanol was rotoevaporated to dryness. The solid was slurred in 20 mL of TBME and filtered. The white solid was dried in a vacuum oven for 5 hours at ˜40° C. 2.08 g of (R)-norfluoxetine (D)-tartrate was obtained (85%). 99.44% ee, 99.53 A % purity. 1H NMR ppm (δ), DMSO 7.63–7.10 (m, 9H), 5.61 (m, 1H, CH—O), 3.90 (dd, 2H), 2.90 (m, 2H), 2.50 (s, 1H), 2.35–2.08 (m, 2H). 13C NMR ppm (δ), DMSO 175.3, 160.8, 140.8, 129.5, 128.71, 127.5, 126.6, 117.0, 77.0, 72.3, 36.4.

1. filtrationfiltered
2. customThe white solid was dried in a vacuum oven for 5 hours at ˜40° C