Sodium Hydroxide → Sodium (4r)-2-[7-({[6-(acetylamino)-2-naphthyl]sulfonyl}amino)-1,1-dioxido-4h-1,2,4-benzothiadiazin-3-yl]-4-methyl-4-(3-methylbutyl)-3-oxo-3,4-dihydronaphthalen-1-olate

Participants

Reaction Steps

A mixture of Example 104A (5.0 mg, 0.0072 mmol) and 0.998 M sodium hydroxide (0.0072 mL, 0.0072 mmol) in water (1 mL) was stirred at rt for 16 h. The reaction mixture was concentrated in vacuo to give the title compound (5.1 mg, quant. yield). 1H NMR (300 MHz, DMSO-d6) δ 0.42 (m, 1H) 0.66 (t, J=6.80 Hz, 6H) 0.75 (m, 1H) 1.26 (m, 1H) 1.36 (s, 3H) 1.73 (m, 1H) 2.10 (m, 4H) 7.21 (d, J=9.93 Hz, 1H) 7.31 (m, J=8.46, 2.21 Hz, 2H) 7.38 (d, J=2.21 Hz, 1H) 7.46 (m, 2H) 7.67 (m, 2H) 8.01 (m, 3H) 8.30 (s, 1H) 8.37 (s, 1H) 10.31 (s, 1H) 10.51 (s, 1H) 15.31 (s, 1H). MS (ESI+) m/z 709.1 (M+H)+, 687.6 (M+H−Na)+, 704.1 (M−Na+NH4)+, (ESI−) m/z 707.1 (M−H)−, 685.0 (M−H−Na)−.

Provenance & Evidence