反应详情

To a stirred solution of the product of Step 1, Example 4 (0.248 g, 0.50 mmol) in CHCl3 (10 mL) is added trifluoroacetic acid (1.1 mL) and stirred the reaction mixture at room temperature for 2 hours. Reaction mixture is concentrated in vacuo and washed the residue with diethyl ether. Residue is dissolved in 10% methanol in CH2Cl2 and evaporated to dryness then dried under vacuum to give the title compound 1H-NMR (400 MHz, DMSO-d6) δ: 4.20-4.22 (m, 1H), 4.28-32 (m, 0.5H), 4.40-4.49 (m, 2.5H), 4.56-4.60 (m, 0.5H), 467-4.71 (m, 0.5H), 4.89 (t, J=3.8 Hz, 1H), 6.02 (d, J=4.28 Hz, 1H), 6.50 (s, 1H), 7.43 (d, J=8.2 Hz, 2H), 7.62 (d, J=8.2 Hz, 2H), 8.28 (s, 1H), 8.48 (bs, 2H), 8.63 (d, J=9 Hz, 1H). m/z (Cl) 392 [M−H].

1. customReaction mixture
2. concentrationis concentrated in vacuo
3. washwashed the residue with diethyl ether
4. dissolutionResidue is dissolved in 10% methanol in CH2Cl2
5. customevaporated to dryness
6. customthen dried under vacuum