反应详情

To a solution of 55A (0.20 g, 0.53 mmol) in DCM (10 mL) was added 70A (0.20 g, 0.93 mmol) followed by DIPEA (0.17 mL, 0.95 mmol). The mixture was stirred at RT for 20 min and then sodium triacetoxyborohydride (0.22 g, 1.05 mmol) was added. The mixture was stirred at RT overnight and then washed with an aqueous solution of Na2CO3. The organic solution was filtered through a phase separator and then the solvent was removed by evaporation. The product was purified on a silica gel column using ethyl acetate and then 5% methanol in DCM where the methanol contained 2M ammonia. There was obtained 128 mg (52%) of 70 as a solid. 1H NMR (500 MHz, CDCl3): δ 0.95 (t, 3H), 1.77 (q, 2H), 3.02 (d, 2H), 3.30 (d, 2H), 3.60 (s, 2H), 3.88 (s, 3H), 4.32 (m, 1H), 4.63 (m, 1H), 4.72 (m, 1H), 5.10 (m, 2H), 6.71 (d, 2H), 7.01 (d, 2H), 7.22 (d, 2H), 8.10 (d, 2H), MS (APCI+) m/z 465 [M+H]+, LC purity: 97%.

1. stirringThe mixture was stirred at RT overnight
2. washwashed with an aqueous solution of Na2CO3
3. filtrationThe organic solution was filtered through a phase separator
4. customthe solvent was removed by evaporation
5. customThe product was purified on a silica gel column