Bromotrimethylsilane → HCID 11525606, compound

Participants

Reaction Steps

Reaction of 1-(1-{2-[(3,3-dimethylbutyl)(ethyl)amino]-2-oxoethyl}-6-methoxy-1H-indazol-3-yl)-2-methylprop-1-en-1-yl dimethyl phosphate with trimethylsilyl bromide as described in Example 2 provided the title compound. It was isolated by RP-HPLC using 10-100% MeCN gradient without TFA as a colorless solid following lyophilization. 1H NMR (CD3CN, 500 MHz) showed two amide rotomers in about 6:7 ratio: δ 7.55 (d, 8.7 Hz, 1H), 6.88 & 6.87 (d, 1.9 Hz, 1H), 6.84 (dd, 2.1 & 8.9 Hz, 1H), 5.23 & 5.21 (s, 2H), 3.88 & 3.87 (s, 3H), 3.31˜3.48 (m, 4H, overlapping with residual water peak), 1.94 (d, 1.8 Hz, 3H), 1.81-1.82 (m, 3H), 1.61-1.64 & 1.42˜1.46 (m, 2H), 1.26 & 1.10 (t, 7.1 Hz, 3H), 0.99 & 0.91 (s, 9H). LC-MS: 3.18 min. (m/Z=370.2, 468.1).

Provenance & Evidence