Réaction #79823

ord-c5c7cbb3195f47909d2a00484a71bb13

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    FiltrationThe precipatate was collected through filtration under nitrogen

Mode opératoire

3-Pyridylmethyl N-[4-(4-amino-7-tetrahydro-2H-4-pyranyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-2-methoxyphenyl]carbamate (12 mg, 0.025 mmol) was dissolved in ethyl acetate (2.0 mL). 1.0N HCl in ether (1 mL) was added slowly. The precipatate was collected through filtration under nitrogen to give 3-pyridylmethyl N-[4-(4-amino-7-tetrahydro-2H-4-pyranyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-2-methoxyphenyl]carbamate hydrochloride(13 mg, 0.25 mmol). 1H NMR (DMSO-d6) δ 1.91 (m, 2H), 2.17 (m, 2H), 3.54 (m, 2H), 3.87 (s, 3H), 4.03 (m, 2H), 4.97 (m, 1H), 5.23 (s, 2H), 7.05 (d, J=8.2 Hz, 1H), 7.13 (s, 1H), 7.51 (m, 1H), 7.81 (d, J=8.2 Hz, 1H), 7.84 (s, 1H), 7.95 (m, 1H), 8.42 (s, 1H), 8.60 (s, 1H), 8.71 (s, 1H), 8.82 (s, 1H). LC/MS MH+=475.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06713474B2uspto-grants-2004_03