反应详情

To a solution of 4-(7H-pyrrolo[2,3-d]pyrimidin-6-yl)-benzoic acid methyl ester (0.601 g, 2.4 mmol) (reference example 43a) in 1:1 THF-methanol (10 mL) is added NaOH (10N) (2.4 mL, 24 mmol) and 0.5 ml H2O. The resulting solution is stirred for 1 hour then cooled to 0°-5° C. and adjusted to pH 3 with 2N HCl. The precipitated solid is filtered off, washed with a small volume of water and dried under high vacuum to give 0.355 g of title compound as a yellow solid. 1H NMR (DMSO) δ 7.59 (s, 1H), 8.10 (d, J=8 Hz, 2H), 8.20 (d, J=8 Hz, 2H), 9.22 (s, 1H), 9.50 (bs, 1H), 14.10 (bs, 1H). MS (EI) m/z 239 (M+).

1. temperaturethen cooled to 0°-5° C.
2. filtrationThe precipitated solid is filtered off
3. washwashed with a small volume of water
4. customdried under high vacuum