Dansyl chloride → HCID 86615486, compound

Participants

Reaction Steps

The product from Example 5 (167 mg, 0.94 mmol) was reacted with 5-Dimethylamino-naphthalene-1-sulfonyl chloride (245 mg, 0.94 mmol) in 10 mL of CH2Cl2 with N,N-diisopropylethylamine (0.530 mL, 410 mmol) for 22 h. Washed with water and dried over Na2SO4, filtered and concentrated under vacuum giving the crude title compound which was purified by HPLC with TFA providing the trifluoroacetic acid salt (35 mg, 40%). 1H NMR (300 MHz, DMSO-d6) δ ppm: 2.75 (s, 3H) 2.86 (s, 6H) 6.65 (d, J=6.99 Hz, 1H) 6.76 (d, J=9.19 Hz, 2H) 6.87 (d, 2H) 7.16 (d, J=8.82 Hz, 1H) 7.34 (d, J=7.72 Hz, 1H) 7.53-7.62 (m, 2H) 7.69-7.79 (m, 3H) 7.97 (d, J=7.35 Hz, 1H) 8.22 (d, J=8.82 Hz, 1H) 8.50 (d, J=6.99 Hz, 1H) 8.60 (d, J=8.46 Hz, 1H) 8.82 (d, J=8.82 Hz, 1H); MS 1H) 8.50 (d, J=6.99 Hz, 1H) 8.60 (d, J=8.46 Hz, 1H) 8.82 (d, J=8.82 Hz, 1H); MS (DCI NH3+) m/z 611 (M+H)+.

Provenance & Evidence