反应详情

温度

22 °C

To a solution of product from step I (370 g, 0.6 mol) in methanol (4,070 mL) in a 12 L round bottom flask equipped with a mechanical stirrer was added L-(+) tartaric acid (90 g, 0.6 mol). The reaction mixture was stirred for about 90 min. at about 22° C., filtered and concentrated. The crude residue was diluted with ethyl acetate (4,560 mL), heated at about 70° C. and slowly allowed to cool to room temperature over about 17 hours. The solid was filtered and dried to give white crystals, mp 188-189° C. (348.46 g, yield 76%). 1H NMR (MeOH, d4) δ: 8.28 (d, 1H), 7.59 (t, 1H), 7.41-7.39 (m, 1H), 7.18-7.13 (m, 1H), 6.92 (t, 1H), 5.2 (t, 1H), 4.56 (bs, 3H), 4.36 (s, 2H), 4.31-4.25 (m, 1H), 4.13-4.06 (m, 1H), 3.78 (d, 2H), 3.21 (t, 1H), 3.18-2.96 (m, 2H), 2.65-2.55 (m, 2H), 1.57 (d, 6H). MS: MH+611. [a]589 +22.03 (c=11.9, MeOH).

1. filtrationfiltered
2. concentrationconcentrated
3. additionThe crude residue was diluted with ethyl acetate (4,560 mL)
4. temperatureheated at about 70° C.
5. temperatureto cool to room temperature over about 17 hours
6. filtrationThe solid was filtered
7. customdried
8. customto give white crystals, mp 188-189° C. (348.46 g, yield 76%)