Trifluoroacetic acid → HCID 86753037, compound

Participants

Reaction Steps

Trifluoroacetic acid (2.0 mL) and 2-(3-{3-[1-(tert-Butoxycarbonyl)-indazol-7-yl]-ureido}-5-methyl-2-oxo-2,3-dihydro-benzo[e][1,4]diazepin-1yl)-N-isopropyl-N-phenyl-acetamide (75 mg, 0.120 mmol), prepared as in Example 4A, are combined, cooled to 0-5--C. with an ice water bath, and stirred under nitrogen for 15 min. The reaction mixture is concentrated in vacuo to an oil, triturated with a mixture of diethyl ether and n-hexane and then concentrated again. This process is repeated several times until a solid is obtained on concentration. The product is dried under high vacuum overnight at room temperature and then at 65--C. overnight to give the title compound as a crystalline solid (61 mg, 0.117 mmol). The pure material is then lyophilized from acetonitrile/water. 1H NMR (300 MHz, CDCl3) δ=1.08-1.12 (m, 6H); 2.73 (s, 3H); 4.11 (d, J=16.8 Hz,1H); 4.24 (d, J=16.6 Hz, 1H); 4.93-5.08 (m, 1H); 5.76 (b, 1H); 6.99-7.75 (m, 14H); 8.00 (b, 1H); 8.83 (b, 1H). MS(FAB): [M+H]+ =524.

Provenance & Evidence