Methyl iodide → HCID 86636300, compound

Participants

Reaction Steps

A solution of 6-chloro-12-piperazin-1-yl-2,4,8,22-tetraazatetracyclo[14.3.1.1(3,7).1(9,13)]docosa-1(20),3(22),4,6,9(21),10,12,16,18-nonaene bis(trifluoroacetate) (20 mg, 32 μmol) and N,N-diisopropylethylamine (27 μL, 0.16 mmol) in dichloromethane (0.3 mL) was treated with methyl iodide (10 μL, 0.16 mmol) and stirred for 16 h. The reaction mixture was purified by preparative LCMS to give the desired product (15 mg, 72%) as a solid. LCMS for C24H28ClN6 (M)+: m/z=435.1. 1H NMR (400 MHz, DMSO-d6): δ 9.41 (s, 1H), 9.17 (s, 1H), 8.11 (s, 1H), 7.98 (s, 1H), 7.81 (d, J=2.3 Hz, 1H), 7.30 (d, J=8.6 Hz, 1H), 7.11-7.07 (m, 2H), 6.87 (d, J=9.2 Hz, 1H), 6.79 (d, J=7.4 Hz, 1H), 3.55-3.53 (m, 4H), 3.22 (s, 6H), 3.15 (br s, 4H), 2.95-2.90 (m, 4H).

Provenance & Evidence