反应详情

Trifluoroacetic acid (25.1 mL) was added to a stirred, chilled (ice-methanol bath) solution of 2-(4-chloro-1-hydroxy-1-indanyl)acetic acid (10.4 g, 0.05 mol) in dichloromethane (230 mL). After 30 min, the mixture was concentrated in vacuo. Dichloromethane was added to the residue and the mixture was concentrated in vacuo to give 6.5 g (68%) of a white solid. Recrystallization of 0.98 g from acetonitrile: 2-propanol mixtures gave 0.62 g of a white solid: m.p., 233°-234° C.; NMR (DMSO-d6): d12.15 (br, 1H, COOH), 7.30-7.81 (m, 3H, Ar), 6.41 (s, 1H, =CH), 3.00-3.06, 3.19-3.22 (2m's, 4H, 2×CH2), steady-state nOe; irradiation at 6.41 d, observed 19.7% nOe at 7.79.

1. concentrationthe mixture was concentrated in vacuo
2. additionDichloromethane was added to the residue
3. concentrationthe mixture was concentrated in vacuo