反应详情

To a solution of (14Z)-6-chloro-2,4,8,22-tetraazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,14,16,18-decaene trifluoroacetate (21 mg, 0.045 mmol) in ethanol (1 mL) was added 5% palladium on carbon (5 mg) and the mixture was purged and degassed with hydrogen three times. The mixture was stirred for 1 hour with balloon pressure of hydrogen. Filtration through celite and purification by preparative LCMS (pH 2) gave the desired product as a trifluoroacetate salt (1.7 mg, 30%). LCMS for C18H16ClN4 (M+H)+: m/z=323.1. 1H NMR (400 MHz, CD3OD): δ 7.75 (m, 2H), 7.30 (m, 1H), 7.22 (m, 1H), 7.12 (m, 1H), 7.03 (m, 2H), 6.90 (m, 1H), 3.00 (s, 4H).

1. customthe mixture was purged
2. customdegassed with hydrogen three times
3. filtrationFiltration
4. customthrough celite and purification by preparative LCMS (pH 2)