Water TFA acetonitrile → HCID 22954742, compound

Participants

Reaction Steps

Compound 2001 (58.6 mg, 0.10 mmol) was treated with 15 mg of TFA/MeCN/water (1:2:3) and stirred at room temperature for 6.5 h. The reaction was extracted with ether. The aqueous layer was concentrated with azeotropic removal of the water using MeCN. The product was suspended in CH2Cl2, concentrated in vacuo and precipitated with ether to give 46.8 mg (99%) of 2002 as a white solid: 1H NMR (CD3OD) δ9.05 (0.25H, d), 8.15 (1H, d), 7.68 (1H, t), 7.64 (0.25H, d), 7.55 (3H, t), 7.35 (0.5H, m), 5.22 (1H, t), 4.90 (1H, m), 4.58 (1H, dd), 4.50 (1H, m), 4.28 (1H, bm), 3.45 (1H, m), 3.10 (1H, bt), 2.68 (1H, ddd), 2.60-2.45 (2H, m), 2.30 (1H, dd), 2.15-2.05 (2H, m), 1.90 (2H, bm), 1.68 (1H, bm).

Provenance & Evidence